CN103505481A - Blood lipid reducing composition containing phytosterol and preparation method of composition - Google Patents
Blood lipid reducing composition containing phytosterol and preparation method of composition Download PDFInfo
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- CN103505481A CN103505481A CN201210217195.6A CN201210217195A CN103505481A CN 103505481 A CN103505481 A CN 103505481A CN 201210217195 A CN201210217195 A CN 201210217195A CN 103505481 A CN103505481 A CN 103505481A
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Abstract
The invention discloses a blood lipid reducing composition containing phytosterol. The composition comprises the following components by weight percent: 5-88% of total flavonoids of sea-buckthorn and 12-95% of phytosterol. The invention also discloses a preparation method of the composition. The preparation method comprises the steps of extracting active ingredients and preparing the finished product according to the formula. The traditional Chinese medicine composition makes the best of the treatment effects of active pharmaceutical ingredients on cardiovascular diseases, adopts scientific matching, generates synergistic effects, has better curative effects and more controllable quality than traditional preparations and is suitable for industrial production.
Description
Technical field
The Chinese medicine composition and the preparation method that the present invention relates to a kind of Cardiovarscular, belong to the field of Chinese medicines.
Background technology
Along with improving constantly of people's living standard, the change of dietary structure, aged tendency of population becomes clear day by day, and the sickness rate of coronary heart disease is day by day soaring.Coronary heart disease is because coronary atherosclerosis causes luminal stenosis, causes blood supply of cardiac muscle oxygen supply obstacle and the heart disease that causes, and " world killer " is known as.With regard to the whole world, since half a century, coronary heart disease has become the underlying cause of death of one of the disease that threat human health the is the most serious ，Shi U.S. and some industrialized country.According to World Health Organization's statistics, in the total death toll of the U.S., have 24.7% to die from coronary heart disease, Northern Ireland coronary heart disease case fatality rate occupies first place in the world, and is 5,36/,100,000; Japan is minimum, is 41,/10 ten thousand.In recent years, the M & M of China's coronary heart disease continues soaring, has every year at present 700,000 people of surpassing to die from coronary heart disease, is the modal a kind of cardiovascular diseases of middle-aged and elderly people, has leapt to as first of internal disease.Visible coronary heart disease has become global public hazards, and American wins cardiopathia for " pestilence in epoch ".
Hyperlipidemia is the risk factor of apoplexy, coronary heart disease, myocardial infarction, sudden death.In addition, hyperlipidemia is also to promote hypertension, an important risk factor of impaired glucose tolerance, diabetes.Hyperlipidemia also can cause fatty liver, liver cirrhosis, cholelithiasis, pancreatitis, retinal hemorrhage, blind, peripheral vascular disease, limping, hyperuricemia.So must pay much attention to the harm of hyperlipidemia, positive prevention and treatment.
Blood lipid-lowering medicine is mainly Statins in the market.Such medicine has good lipid-lowering effect, but long-term taking, can be just like myalgia, muscle inflammation, even the musclar toxicity such as rhabdomyolysis, also can produce the side effect such as internal metabolism obstacle, gastrointestinal side effect, liver loss.Meanwhile, statins price is high, and long-term taking also can the corresponding financial burden that increases patient.
So, provide controlled, cheap, the eutherapeutic pure natural plant of a kind of safety to extract medicine, there is great social meaning and economic worth.
Summary of the invention
The object of the invention is a kind of good effect, the more controlled Chinese medicine composition of quality.
Another object of the present invention is a kind of preparation method of described Chinese medicine composition.
Another object of the present invention is to provide a kind ofly has the Chinese medicine composition of the market competitiveness in price equally.Described Chinese medicine composition can not increase because of the raising of curative effect patient's financial burden.
For achieving the above object, the present invention by the following technical solutions:
In Chinese medicine composition of the present invention, comprise the component of following percentage by weight:
Fructus Hippophae total flavones 5～88%, plant sterol 12～95%;
Preferably, in Chinese medicine composition of the present invention, comprise the component of following percentage by weight:
Fructus Hippophae total flavones 18～72%, plant sterol 28～82%;
Preferred, in Chinese medicine composition of the present invention, comprise the component of following percentage by weight:
Fructus Hippophae total flavones 40～60%, plant sterol 40～60%;
Further preferred, in Chinese medicine composition of the present invention, comprise the component of following percentage by weight:
Fructus Hippophae total flavones 45%, plant sterol 55%.
Described Fructus Hippophae total flavones can be buied from open market, also can adopt following preparation method to obtain.
In pharmaceutical composition of the present invention, the extracting method of Fructus Hippophae total flavones, comprises the steps:
Get Fructus Hippophae medical material, after being pulverized, add ethyl acetate and ethanol, heating and refluxing extraction, obtain extracting solution I, medicinal residues add ethanol, and heating and refluxing extraction obtains extracting solution II, merge extractive liquid, I and II, be condensed into extractum, use dissolve with ethanol extractum, adopt nonpolar or low pole macroporous resin to carry out separation to it, first with water elution, obtain eluent I; Then with ethanol elution 2 times, the volumetric concentration of eluting ethanol is 50%～60% for the first time, and the volumetric concentration of eluting ethanol is 90%～95% for the second time, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract;
Preferably, the volume ratio of described ethyl acetate and ethanol is 1:2.
Preferably, the volumetric concentration of eluting ethanol is 60% for the first time; The volumetric concentration of eluting ethanol is 90% for the second time.
Preferred, in Chinese medicine composition of the present invention, the preparation method of Fructus Hippophae total flavones comprises the following steps:
Get Fructus Hippophae medical material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 1～3 hour for the first time, 1～2 hour for the second time, filtrate merged to obtain extracting solution I, and medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 0.5～1.5 hour for the first time, 0.5～1 hour for the second time, filtrate merged to obtain extracting solution II, merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopt nonpolar or low pole macroporous resin to carry out separation to it, first with water elution, obtain eluent I; Then with 50%～60% ethanol elution, then with 90%～95% ethanol elution, obtain eluent II, reclaim, concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract;
Described elution flow rate is 1～4BV/h; Preferably, elution flow rate is 1～2BV/h, is more preferably 2BV/h.
Described macroporous resin is preferably AB～8 and X～5, more preferably X～5.
After testing, Fructus Hippophae total flavones product purity can reach 24～26%.
Concentration of alcohol described in the present invention is volumetric concentration.
In pharmaceutical composition of the present invention, plant sterol can be buied from open market, also can adopt following method preparation.
In pharmaceutical composition of the present invention, the extracting method of plant sterol, comprises the steps:
(1) extract: raw material drying, to pulverize, petroleum ether is or/and ethyl acetate heats 56～70 ℃ of reflux, extract,, and extracting solution concentrating under reduced pressure, obtains extractum (containing solute 40～45%);
(2) column chromatography: by gained condensed cream to etc. on the chromatographic column of weight silica gel, first use petroleum ether: ethyl acetate=95:5 as mobile phase, obtain eluent I, then change petroleum ether: ethyl acetate=85:15 as mobile phase, obtain eluent II;
Flow velocity 0.2～2BV/h, preferred, 0.5～1 BV/h.
(3) crystallization: eluent II air-distillation is concentrated, when being concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystal crude product, reclaims solvent;
Through high performance liquid chromatogram (HPLC), detect, in crystallization, sterol content 94.04～97.27%.
(4) recrystallization: by crystal crude product petroleum ether: ethyl acetate=85:15 mixed solvent heating for dissolving, filtration, when filtrate has been concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystalline product.
Through high performance liquid chromatogram (HPLC), detect, in crystallization, sterol content 97.05～99.01%.
Developing solvent system is petroleum ether: ethyl acetate=85:15; Lamellae is: silica gel G thin layer chromatography silica gel; Thin layer specification: 10cm * 10cm, thickness 0.1mm.
The extraction raw material of sterol of the present invention includes but not limited to Semen Maydis, Semen sojae atricolor, Semen arachidis hypogaeae, Semen Sesami, Fructus Hippophae.Preferably Semen Maydis and Fructus Hippophae.
Solve technological process elapsed time (48～54 hours) for a long time, the problem that industrial production efficiency is low.Sterol extracting method eluent composition of the present invention is simple, cost is low, is beneficial to suitability for industrialized production.
Described dosage form can be the various dosage forms that on Chinese medicine composition of the present invention and any or more than one pharmaceuticss, adjuvant is mixed as starch, dextrin, lactose, microcrystalline Cellulose, hydroxypropyl methylcellulose, Polyethylene Glycol, magnesium stearate, micropowder silica gel, xylitol, lactose, glucose, glycine, mannitol, glycine etc., for example, can be made into aqueous injection, tablet, slow releasing tablet, drop pill, granule, injectable powder, capsule, microgranule.Preferred dosage form is drop pill, injectable powder.
Chinese medicine composition of the present invention can also adopt following method to realize:
Chinese medicine composition purity of the present invention is high, dosage is little, and more traditional Fructus Hippophae total flavones extract formulation has better curative effect, and quality is more controlled, can reduce patient suffering and financial burden.
test example
Medicine blood fat reducing clinical observation of the present invention
1. data and method
1.1 physical data are selected hyperlipidemia patient 80 examples at random, male 40 examples, and female's 40 examples, at 46～74 years old age, average 57.4 years old, selecting 80 routine hyperlipidemia patients else was matched group, male 41 examples, female's 39 examples, 42～76 years old age, 58.7 years old mean age.
1.2 administrated method
Treatment group adopts the embodiment of the present invention 4 medicines, each 10mg, oral 3 times of every day, 2 months courses for the treatment of.Matched group gives Xuezhikang, each 10mg, every day 3 times, 2 months courses for the treatment of.Before treatment, withdraw other hypolipidemic.All patients before treatment, treatment does hematuria routine, blood fat, liver function, renal function, serum potassium, uranium, chlorine, blood glucose, Electrocardioscopy after January and the course for the treatment of finishing.
1.3 observation item
Before and after treatment, take out limosis vein blood and detect serum total cholesterol (TC), triglyceride (TG), high density lipoprotein (HDL～C), low density lipoprotein, LDL (LDL～C), do liver function, renal function, blood, urine routine test simultaneously.
1.4 statistical procedures
Mean ± standard deviation for measurement data (
) represent, adopt t check; Enumeration data x
2check, P < 0.05 has significance for difference.
2. result
The curative effect of hyperlipidemia
Before and after table 1 liang group lipid therapy, compare (
)
Note: before and after * group internal therapy than P < 0.05, between # group after treatment than P < 0.05.
The present invention and Xuezhikang all have lipid-lowering effect, and present composition lipid-lowering effect is better than Xuezhikang.
The specific embodiment
embodiment 1
(1) sterol extracts
Raw material drying, pulverizes, and petroleum ether is or/and ethyl acetate heats 56 ℃ of reflux, extract,, and extracting solution concentrating under reduced pressure, obtains extractum (containing solute 40%); By on gained condensed cream to etc. on the chromatographic column of weight silica gel, first use petroleum ether: ethyl acetate=95:5 as mobile phase, obtain eluent I, then change petroleum ether: ethyl acetate=85:15 as mobile phase, flow velocity 2BV/h, obtains eluent II; Eluent II air-distillation is concentrated, and when being concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystal crude product, reclaims solvent; By crystal crude product petroleum ether: ethyl acetate=85:15 mixed solvent heating for dissolving, filtration, when filtrate has been concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystalline product.After testing, sterol content 97.05% in crystallization.
(2) Fructus Hippophae total flavones extracts
Get Fructus Hippophae medical material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 1.5 hours for the first time, 1 hour for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1 hour for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with methanol extractum, adopts macroporous resin AB～8 to carry out separation, first with water elution, obtains eluent I; Then with 55% ethanol elution, then with 90% ethanol elution, eluent flow rate is 2.5BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract.
Get above-mentioned Fructus Hippophae total flavones extract 5%, steroidal extract 95%, adds adjuvant and is prepared into Chinese medicine composition of the present invention.
embodiment 2
(1) sterol extracts
Raw material drying, pulverizes, and petroleum ether is or/and ethyl acetate heats 70 ℃ of reflux, extract,, and extracting solution concentrating under reduced pressure, obtains extractum (containing solute 40%); By on gained condensed cream to etc. on the chromatographic column of weight silica gel, first use petroleum ether: ethyl acetate=95:5 as mobile phase, obtain eluent I, then change petroleum ether: ethyl acetate=85:15 as mobile phase, flow velocity 0.2BV/h obtains eluent II; Eluent II air-distillation is concentrated, and when being concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystal crude product, reclaims solvent; By crystal crude product petroleum ether: ethyl acetate=85:15 mixed solvent heating for dissolving, filtration, when filtrate has been concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystalline product.Through high performance liquid chromatogram (HPLC), detect, in crystallization, sterol content 97.15%.
(2) Fructus Hippophae total flavones extracts
Get Fructus Hippophae medical material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 1.5 hours for the first time, 1 hour for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1 hour for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with methanol extractum, adopts macroporous resin X～5 to carry out separation, first with water elution, obtains eluent I; Then with 60% ethanol elution, then with 95% ethanol elution, eluent flow rate is 2BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract.
Get above-mentioned Fructus Hippophae total flavones extract 88%, steroidal extract 12%, adds adjuvant and is prepared into Chinese medicine composition of the present invention.
embodiment 3
(1) sterol extracts
Raw material drying, pulverizes, and petroleum ether is or/and ethyl acetate heats 60 ℃ of reflux, extract,, and extracting solution concentrating under reduced pressure, obtains extractum (containing solute 45%); By on gained condensed cream to etc. on the chromatographic column of weight silica gel, first use petroleum ether: ethyl acetate=95:5 as mobile phase, obtain eluent I, then change petroleum ether: ethyl acetate=85:15 as mobile phase, flow velocity 2BV/h, obtains eluent II; Eluent II air-distillation is concentrated, and when being concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystal crude product, reclaims solvent; By crystal crude product petroleum ether: ethyl acetate=85:15 mixed solvent heating for dissolving, filtration, when filtrate has been concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystalline product.After testing, sterol content 97.21% in crystallization.
(2) Fructus Hippophae total flavones extracts
Get Fructus Hippophae medical material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 2 hours for the first time, 1 hour for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1 hour for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin X～5 to carry out separation, first with water elution, obtains eluent I; Then with 55% ethanol elution, then with 95% ethanol elution, eluent flow rate is 2BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract.
Get above-mentioned Fructus Hippophae total flavones extract 18%, steroidal extract 82%, adds adjuvant and is prepared into Chinese medicine composition of the present invention.
embodiment 4
(1) sterol extracts
Raw material drying, pulverizes, and petroleum ether is or/and ethyl acetate heats 65 ℃ of reflux, extract,, and extracting solution concentrating under reduced pressure, obtains extractum (containing solute 45%); By on gained condensed cream to etc. on the chromatographic column of weight silica gel, first use petroleum ether: ethyl acetate=95:5 as mobile phase, obtain eluent I, then change petroleum ether: ethyl acetate=85:15 as mobile phase, flow velocity 1 BV/h, obtains eluent II; Eluent II air-distillation is concentrated, and when being concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystal crude product, reclaims solvent; By crystal crude product petroleum ether: ethyl acetate=85:15 mixed solvent heating for dissolving, filtration, when filtrate has been concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystalline product.After testing, sterol content 99.01% in crystallization.
(2) Fructus Hippophae total flavones extracts
Get Fructus Hippophae medical material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 1 hour for the first time, 1 hour for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 0.5 hour for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin AB～8 to carry out separation, first with water elution, obtains eluent I; Then with 50% ethanol elution, then with 90% ethanol elution, eluent flow rate is 1BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract.
Get above-mentioned Fructus Hippophae total flavones extract 45%, steroidal extract 55%, adds adjuvant and is prepared into Chinese medicine composition of the present invention.
embodiment 5
(1) sterol extracts
Raw material drying, pulverizes, and petroleum ether is or/and ethyl acetate heats 60 ℃ of reflux, extract,, and extracting solution concentrating under reduced pressure, obtains extractum (containing solute 40%); By on gained condensed cream to etc. on the chromatographic column of weight silica gel, first use petroleum ether: ethyl acetate=95:5 as mobile phase, obtain eluent I, then change petroleum ether: ethyl acetate=85:15 as mobile phase, flow velocity 0.5BV/h, obtains eluent II; Eluent II air-distillation is concentrated, and when being concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystal crude product, reclaims solvent; By crystal crude product petroleum ether: ethyl acetate=85:15 mixed solvent heating for dissolving, filtration, when filtrate has been concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystalline product.After testing, sterol content 98.01% in crystallization.
(2) Fructus Hippophae total flavones extracts
Get Fructus Hippophae medical material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 3 hours for the first time, 2 hours for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1.5 hours for the first time, 1 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin X～5 to carry out separation, first with water elution, obtains eluent I; Then with 60% ethanol elution, then with 95% ethanol elution, eluent flow rate is 4BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract.
Get above-mentioned Fructus Hippophae total flavones extract 72%, steroidal extract 28%, adds adjuvant and is prepared into Chinese medicine composition of the present invention.
embodiment 6
(1) sterol extracts
Raw material drying, pulverizes, and petroleum ether is or/and ethyl acetate heats 70 ℃ of reflux, extract,, and extracting solution concentrating under reduced pressure, obtains extractum (containing solute 45%); By on gained condensed cream to etc. on the chromatographic column of weight silica gel, first use petroleum ether: ethyl acetate=95:5 as mobile phase, obtain eluent I, then change petroleum ether: ethyl acetate=85:15 as mobile phase, flow velocity 1.5BV/h, obtains eluent II; Eluent II air-distillation is concentrated, and when being concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystal crude product, reclaims solvent; By crystal crude product petroleum ether: ethyl acetate=85:15 mixed solvent heating for dissolving, filtration, when filtrate has been concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystalline product.After testing, sterol content 98.11% in crystallization.
(2) Fructus Hippophae total flavones extracts
Get Fructus Hippophae medical material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 1.5 hours for the first time, 1 hour for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1 hour for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin X～5 to carry out separation, first with water elution, obtains eluent I; Then with 55% ethanol elution, then with 90% ethanol elution, eluent flow rate is 2BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract.
Get above-mentioned Fructus Hippophae total flavones extract 40%, steroidal extract 60%, adds adjuvant and is prepared into Chinese medicine composition of the present invention.
embodiment 7
(1) sterol extracts
Raw material drying, pulverizes, and petroleum ether is or/and ethyl acetate heats 65 ℃ of reflux, extract,, and extracting solution concentrating under reduced pressure, obtains extractum (containing solute 42%); By on gained condensed cream to etc. on the chromatographic column of weight silica gel, first use petroleum ether: ethyl acetate=95:5 as mobile phase, obtain eluent I, then change petroleum ether: ethyl acetate=85:15 as mobile phase, flow velocity 1 BV/h, obtains eluent II; Eluent II air-distillation is concentrated, and when being concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystal crude product, reclaims solvent; By crystal crude product petroleum ether: ethyl acetate=85:15 mixed solvent heating for dissolving, filtration, when filtrate has been concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystalline product.After testing, sterol content 98.18% in crystallization.
(2) Fructus Hippophae total flavones extracts
Get Fructus Hippophae medical material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 2 hours for the first time, 1 hour for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1.5 hours for the first time, 1 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin X～5 to carry out separation, first with water elution, obtains eluent I; Then with 60% ethanol elution, then with 95% ethanol elution, eluent flow rate is 3BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract.
Get above-mentioned Fructus Hippophae total flavones extract 60%, steroidal extract 40%, adds adjuvant and is prepared into Chinese medicine composition of the present invention.
embodiment 8
(1) sterol extracts
Raw material drying, pulverizes, and petroleum ether is or/and ethyl acetate heats 68 ℃ of reflux, extract,, and extracting solution concentrating under reduced pressure, obtains extractum (containing solute 44%); By on gained condensed cream to etc. on the chromatographic column of weight silica gel, first use petroleum ether: ethyl acetate=95:5 as mobile phase, obtain eluent I, then change petroleum ether: ethyl acetate=85:15 as mobile phase, flow velocity 1 BV/h, obtains eluent II; Eluent II air-distillation is concentrated, and when being concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystal crude product, reclaims solvent; By crystal crude product petroleum ether: ethyl acetate=85:15 mixed solvent heating for dissolving, filtration, when filtrate has been concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystalline product.After testing, sterol content 98.33% in crystallization.
(2) Fructus Hippophae total flavones extracts
Get Fructus Hippophae medical material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 2 hours for the first time, 2 hours for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1.5 hours for the first time, 1 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin AB～8 to carry out separation, first with water elution, obtains eluent I; Then with 50% ethanol elution, then with 90% ethanol elution, eluent flow rate is 2BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract.
Get above-mentioned Fructus Hippophae total flavones extract 85%, steroidal extract 15%, adds adjuvant and is prepared into Chinese medicine composition of the present invention.
embodiment 9
(1) sterol extracts
Raw material drying, pulverizes, and petroleum ether is or/and ethyl acetate heats 64 ℃ of reflux, extract,, and extracting solution concentrating under reduced pressure, obtains extractum (containing solute 43%); By on gained condensed cream to etc. on the chromatographic column of weight silica gel, first use petroleum ether: ethyl acetate=95:5 as mobile phase, obtain eluent I, then change petroleum ether: ethyl acetate=85:15 as mobile phase, flow velocity 1.5 BV/h, obtain eluent II; Eluent II air-distillation is concentrated, and when being concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystal crude product, reclaims solvent; By crystal crude product petroleum ether: ethyl acetate=85:15 mixed solvent heating for dissolving, filtration, when filtrate has been concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystalline product.After testing, sterol content 97.88% in crystallization.
(2) Fructus Hippophae total flavones extracts
Get Fructus Hippophae medical material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 1.5 hours for the first time, 1.5 hours for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1 hour for the first time, 1 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin 1X～5 to carry out separation, first with water elution, obtains eluent I; Then with 55% ethanol elution, then with 95% ethanol elution, eluent flow rate is 2.5BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract.
Get above-mentioned Fructus Hippophae total flavones extract 75%, steroidal extract 25%, adds adjuvant and is prepared into Chinese medicine composition of the present invention.
embodiment 10
(1) sterol extracts
Raw material drying, pulverizes, and petroleum ether is or/and ethyl acetate heats 68 ℃ of reflux, extract,, and extracting solution concentrating under reduced pressure, obtains extractum (containing solute 45%); By on gained condensed cream to etc. on the chromatographic column of weight silica gel, first use petroleum ether: ethyl acetate=95:5 as mobile phase, obtain eluent I, then change petroleum ether: ethyl acetate=85:15 as mobile phase, flow velocity 0.2BV/h, obtains eluent II; Eluent II air-distillation is concentrated, and when being concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystal crude product, reclaims solvent; By crystal crude product petroleum ether: ethyl acetate=85:15 mixed solvent heating for dissolving, filtration, when filtrate has been concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystalline product.After testing, sterol content 98.76% in crystallization.
(2) Fructus Hippophae total flavones extracts
Get Fructus Hippophae medical material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 3 hours for the first time, 2 hours for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1.5 hours for the first time, 1 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin X～5 to carry out separation, first with water elution, obtains eluent I; Then with 55% ethanol elution, then with 95% ethanol elution, eluent flow rate is 2BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract.
Get above-mentioned Fructus Hippophae total flavones extract 70%, steroidal extract 30%, adds adjuvant and is prepared into Chinese medicine composition of the present invention.
embodiment 11
(1) sterol extracts
Raw material drying, pulverizes, and petroleum ether is or/and ethyl acetate heats 58 ℃ of reflux, extract,, and extracting solution concentrating under reduced pressure, obtains extractum (containing solute 40%); By on gained condensed cream to etc. on the chromatographic column of weight silica gel, first use petroleum ether: ethyl acetate=95:5 as mobile phase, obtain eluent I, then change petroleum ether: ethyl acetate=85:15 as mobile phase, flow velocity 0.5BV/h, obtains eluent II; Eluent II air-distillation is concentrated, and when being concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystal crude product, reclaims solvent; By crystal crude product petroleum ether: ethyl acetate=85:15 mixed solvent heating for dissolving, filtration, when filtrate has been concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystalline product.After testing, sterol content 98.66% in crystallization.
(2) Fructus Hippophae total flavones extracts
Get Fructus Hippophae medical material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 2.5 hours for the first time, 1.5 hours for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1 hour for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin AB～8 to carry out separation, first with water elution, obtains eluent I; Then with 60% ethanol elution, then with 95% ethanol elution, eluent flow rate is 3.5BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract.
Get above-mentioned Fructus Hippophae total flavones extract 64%, steroidal extract 36%, adds adjuvant and is prepared into Chinese medicine composition of the present invention.
embodiment 12
(1) sterol extracts
Raw material drying, pulverizes, and petroleum ether is or/and ethyl acetate heats 70 ℃ of reflux, extract,, and extracting solution concentrating under reduced pressure, obtains extractum (containing solute 40%); By on gained condensed cream to etc. on the chromatographic column of weight silica gel, first use petroleum ether: ethyl acetate=95:5 as mobile phase, obtain eluent I, then change petroleum ether: ethyl acetate=85:15 as mobile phase, flow velocity 0.6BV/h, obtains eluent II; Eluent II air-distillation is concentrated, and when being concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystal crude product, reclaims solvent; By crystal crude product petroleum ether: ethyl acetate=85:15 mixed solvent heating for dissolving, filtration, when filtrate has been concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystalline product.Through high performance liquid chromatogram (HPLC), detect, in crystallization, sterol content 98.45%.
(2) Fructus Hippophae total flavones extracts
Get Fructus Hippophae medical material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 2.5 hours for the first time, 1.5 hours for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1.5 hours for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin X～5 to carry out separation, first with water elution, obtains eluent I; Then with 54% ethanol elution, then with 93% ethanol elution, eluent flow rate is 4BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract.
Get above-mentioned Fructus Hippophae total flavones extract 55%, steroidal extract 45%, adds adjuvant and is prepared into Chinese medicine composition of the present invention.
embodiment 13
(1) sterol extracts
Raw material drying, pulverizes, and petroleum ether is or/and ethyl acetate heats 59 ℃ of reflux, extract,, and extracting solution concentrating under reduced pressure, obtains extractum (containing solute 44%); By on gained condensed cream to etc. on the chromatographic column of weight silica gel, first use petroleum ether: ethyl acetate=95:5 as mobile phase, obtain eluent I, then change petroleum ether: ethyl acetate=85:15 as mobile phase, flow velocity 1BV/h, obtains eluent II; Eluent II air-distillation is concentrated, and when being concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystal crude product, reclaims solvent; By crystal crude product petroleum ether: ethyl acetate=85:15 mixed solvent heating for dissolving, filtration, when filtrate has been concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystalline product.After testing, sterol content 97. 99% in crystallization.
(2) Fructus Hippophae total flavones extracts
Get Fructus Hippophae medical material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 3 hours for the first time, 1 hour for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 0.5 hour for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin X～5 to carry out separation, first with water elution, obtains eluent I; Then with 59% ethanol elution, then with 94% ethanol elution, eluent flow rate is 3.5BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract.
Get above-mentioned Fructus Hippophae total flavones extract 50%, steroidal extract 50%, adds adjuvant and is prepared into Chinese medicine composition of the present invention.
embodiment 14
(1) sterol extracts
Raw material drying, pulverizes, and petroleum ether is or/and ethyl acetate heats 56 ℃ of reflux, extract,, and extracting solution concentrating under reduced pressure, obtains extractum (containing solute 41%); By on gained condensed cream to etc. on the chromatographic column of weight silica gel, first use petroleum ether: ethyl acetate=95:5 as mobile phase, obtain eluent I, then change petroleum ether: ethyl acetate=85:15 as mobile phase, flow velocity 0.8BV/h, obtains eluent II; Eluent II air-distillation is concentrated, and when being concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystal crude product, reclaims solvent; By crystal crude product petroleum ether: ethyl acetate=85:15 mixed solvent heating for dissolving, filtration, when filtrate has been concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystalline product.After testing, sterol content 98.71% in crystallization.
(2) Fructus Hippophae total flavones extracts
Get Fructus Hippophae medical material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 1 hour for the first time, 1 hour for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 0.5 hour for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin AB～8 to carry out separation, first with water elution, obtains eluent I; Then with 58% ethanol elution, then with 92% ethanol elution, eluent flow rate is 1.5BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract.
Get above-mentioned Fructus Hippophae total flavones extract 45%, steroidal extract 55%, adds adjuvant and is prepared into Chinese medicine composition of the present invention.
embodiment 15
(1) sterol extracts
Raw material drying, pulverizes, and petroleum ether is or/and ethyl acetate heats 60 ℃ of reflux, extract,, and extracting solution concentrating under reduced pressure, obtains extractum (containing solute 45%); By on gained condensed cream to etc. on the chromatographic column of weight silica gel, first use petroleum ether: ethyl acetate=95:5 as mobile phase, obtain eluent I, then change petroleum ether: ethyl acetate=85:15 as mobile phase, flow velocity 2BV/h, obtains eluent II; Eluent II air-distillation is concentrated, and when being concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystal crude product, reclaims solvent; By crystal crude product petroleum ether: ethyl acetate=85:15 mixed solvent heating for dissolving, filtration, when filtrate has been concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystalline product.After testing, sterol content 98.40% in crystallization.
(2) Fructus Hippophae total flavones extracts
Get Fructus Hippophae medical material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 1.5 hours for the first time, 1 hour for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1.5 hours for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin X～5 to carry out separation, first with water elution, obtains eluent I; Then with 55% ethanol elution, then with 95% ethanol elution, eluent flow rate is 2.5BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract.
Get above-mentioned Fructus Hippophae total flavones extract 35%, steroidal extract 65%, adds adjuvant and is prepared into Chinese medicine composition of the present invention.
embodiment 16
(1) sterol extracts
Raw material drying, pulverizes, and petroleum ether is or/and ethyl acetate heats 70 ℃ of reflux, extract,, and extracting solution concentrating under reduced pressure, obtains extractum (containing solute 45%); By on gained condensed cream to etc. on the chromatographic column of weight silica gel, first use petroleum ether: ethyl acetate=95:5 as mobile phase, obtain eluent I, then change petroleum ether: ethyl acetate=85:15 as mobile phase, flow velocity 2BV/h, obtains eluent II; Eluent II air-distillation is concentrated, and when being concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystal crude product, reclaims solvent; By crystal crude product petroleum ether: ethyl acetate=85:15 mixed solvent heating for dissolving, filtration, when filtrate has been concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystalline product.After testing, sterol content 97.69% in crystallization.
(2) Fructus Hippophae total flavones extracts
Get Fructus Hippophae medical material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 3 hours for the first time, 2 hours for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1 hour for the first time, 1 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin AB～8 to carry out separation, first with water elution, obtains eluent I; Then with 50% ethanol elution, then with 95% ethanol elution, eluent flow rate is 3BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract.
Get above-mentioned Fructus Hippophae total flavones extract 25%, steroidal extract 75%, adds adjuvant and is prepared into Chinese medicine composition of the present invention.
embodiment 17
(1) sterol extracts
Raw material drying, pulverizes, and petroleum ether is or/and ethyl acetate heats 56～70 ℃ of reflux, extract,, and extracting solution concentrating under reduced pressure, obtains extractum (containing solute 40～45%); By on gained condensed cream to etc. on the chromatographic column of weight silica gel, first use petroleum ether: ethyl acetate=95:5 as mobile phase, obtain eluent I, then change petroleum ether: ethyl acetate=85:15 as mobile phase, flow velocity 2BV/h, obtains eluent II; Eluent II air-distillation is concentrated, and when being concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystal crude product, reclaims solvent; By crystal crude product petroleum ether: ethyl acetate=85:15 mixed solvent heating for dissolving, filtration, when filtrate has been concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystalline product.After testing, sterol content 97.52% in crystallization.
(2) Fructus Hippophae total flavones extracts
Get Fructus Hippophae medical material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 2.5 hours for the first time, 1 hour for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1 hour for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin X～5 to carry out separation, first with water elution, obtains eluent I; Then with 60% ethanol elution, then with 90% ethanol elution, eluent flow rate is 1BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract.
Get above-mentioned Fructus Hippophae total flavones extract 20%, steroidal extract 80%, adds adjuvant and is prepared into Chinese medicine composition of the present invention.
embodiment 18
(1) sterol extracts
Raw material drying, pulverizes, and petroleum ether is or/and ethyl acetate heats 56 ℃ of reflux, extract,, and extracting solution concentrating under reduced pressure, obtains extractum (containing solute 40%); By on gained condensed cream to etc. on the chromatographic column of weight silica gel, first use petroleum ether: ethyl acetate=95:5 as mobile phase, obtain eluent I, then change petroleum ether: ethyl acetate=85:15 as mobile phase, flow velocity 0.3BV/h, obtains eluent II; Eluent II air-distillation is concentrated, and when being concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystal crude product, reclaims solvent; By crystal crude product petroleum ether: ethyl acetate=85:15 mixed solvent heating for dissolving, filtration, when filtrate has been concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystalline product.After testing, sterol content 97.81% in crystallization.
(2) Fructus Hippophae total flavones extracts
Get Fructus Hippophae medical material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, heating and refluxing extraction 2 times, 3 hours for the first time, 2 hours for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 1.5 hours for the first time, 0.5 hour for the second time, filtrate merged to obtain extracting solution II; Merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopts macroporous resin AB～8 to carry out separation, first with water elution, obtains eluent I; Then with 50% ethanol elution, then with 95% ethanol elution, eluent flow rate is 1BV/h, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract.
Get above-mentioned Fructus Hippophae total flavones extract 10%, steroidal extract 90%, adds adjuvant and is prepared into Chinese medicine composition of the present invention.
embodiment 19
(1) sterol extracts
Raw material drying, pulverizes, and petroleum ether is or/and ethyl acetate heats 58 ℃ of reflux, extract,, and extracting solution concentrating under reduced pressure, obtains extractum (containing solute 42%); By on gained condensed cream to etc. on the chromatographic column of weight silica gel, first use petroleum ether: ethyl acetate=95:5 as mobile phase, obtain eluent I, then change petroleum ether: ethyl acetate=85:15 as mobile phase, flow velocity 0.8BV/h, obtains eluent II; Eluent II air-distillation is concentrated, and when being concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystal crude product, reclaims solvent; By crystal crude product petroleum ether: ethyl acetate=85:15 mixed solvent heating for dissolving, filtration, when filtrate has been concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystalline product.After testing, sterol content 98.70% in crystallization.
(2) Fructus Hippophae total flavones extracts
Get Fructus Hippophae medical material, after being pulverized, add ethyl acetate and ethanol, heating and refluxing extraction, obtain extracting solution I, medicinal residues add ethanol, and heating and refluxing extraction obtains extracting solution II, merge extractive liquid, I and II, be condensed into extractum, use dissolve with ethanol extractum, adopt macroporous resin X～5 to carry out separation to it, first with water elution, obtain eluent I; Then with ethanol elution 2 times, the volumetric concentration of eluting ethanol is 60% for the first time, and the volumetric concentration of eluting ethanol is 90%% for the second time, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract.
Get above-mentioned Fructus Hippophae total flavones extract 8%, steroidal extract 92%, adds adjuvant and is prepared into Chinese medicine composition of the present invention.
embodiment 20
(1) sterol extracts
Raw material drying, pulverizes, and petroleum ether is or/and ethyl acetate heats 65 ℃ of reflux, extract,, and extracting solution concentrating under reduced pressure, obtains extractum (containing solute 40%); By on gained condensed cream to etc. on the chromatographic column of weight silica gel, first use petroleum ether: ethyl acetate=95:5 as mobile phase, obtain eluent I, then change petroleum ether: ethyl acetate=85:15 as mobile phase, flow velocity 1.5BV/h, obtains eluent II; Eluent II air-distillation is concentrated, and when being concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystal crude product, reclaims solvent; By crystal crude product petroleum ether: ethyl acetate=85:15 mixed solvent heating for dissolving, filtration, when filtrate has been concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystalline product.After testing, sterol content 98.95% in crystallization.
(2) Fructus Hippophae total flavones extracts
Get Fructus Hippophae medical material, after being pulverized, add ethyl acetate and the ethanol of volume ratio 1:2, heating and refluxing extraction, obtain extracting solution I, medicinal residues add ethanol, and heating and refluxing extraction obtains extracting solution II, merge extractive liquid, I and II, be condensed into extractum, use dissolve with ethanol extractum, adopt macroporous resin AB～8 to carry out separation to it, first with water elution, obtain eluent I; Then with ethanol elution 2 times, the volumetric concentration of eluting ethanol is 55% for the first time, and the volumetric concentration of eluting ethanol is 95% for the second time, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract.
Get above-mentioned Fructus Hippophae total flavones extract 66%, steroidal extract 44%, adds adjuvant and is prepared into Chinese medicine composition of the present invention.
embodiment 21
(1) sterol extracts
Raw material drying, pulverizes, and petroleum ether is or/and ethyl acetate heats 64 ℃ of reflux, extract,, and extracting solution concentrating under reduced pressure, obtains extractum (containing solute 45%); By on gained condensed cream to etc. on the chromatographic column of weight silica gel, first use petroleum ether: ethyl acetate=95:5 as mobile phase, obtain eluent I, then change petroleum ether: ethyl acetate=85:15 as mobile phase, flow velocity 1BV/h, obtains eluent II; Eluent II air-distillation is concentrated, and when being concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystal crude product, reclaims solvent; By crystal crude product petroleum ether: ethyl acetate=85:15 mixed solvent heating for dissolving, filtration, when filtrate has been concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystalline product.After testing, sterol content 98.80% in crystallization.
(2) Fructus Hippophae total flavones extracts
Get Fructus Hippophae medical material, after being pulverized, add ethyl acetate and the ethanol of volume ratio 1:2, heating and refluxing extraction, obtain extracting solution I, medicinal residues add ethanol, and heating and refluxing extraction obtains extracting solution II, merge extractive liquid, I and II, be condensed into extractum, use dissolve with ethanol extractum, adopt macroporous resin X～5 to carry out separation to it, first with water elution, obtain eluent I; Then with ethanol elution 2 times, the volumetric concentration of eluting ethanol is 60% for the first time, and the volumetric concentration of eluting ethanol is 90% for the second time, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract.
Take by weight above-mentioned Fructus Hippophae total flavones extract 68%, steroidal extract 32%, adds adjuvant and is prepared into Chinese medicine composition of the present invention.
Chinese medicine composition disclosed by the invention, those skilled in the art can extract link by change and realize.Embodiments of the invention are only the specific descriptions to technical scheme, are not the restrictions to technical scheme, and those skilled in the art all fall into protection scope of the present invention not changing the replacement done under the condition of flesh and blood of the present invention or change.
Claims (10)
1. a compositions that contains sterol, comprises the component of following percentage by weight: Fructus Hippophae total flavones 5～88%, plant sterol 12～95%.
2. compositions according to claim 1, is characterized in that, described weight percentages of components is: Fructus Hippophae total flavones 18～72%, plant sterol 28～82%.
3. compositions according to claim 2, is characterized in that, described weight percentages of components is: Fructus Hippophae total flavones 40～60%, plant sterol 40～60%.
4. compositions according to claim 3, is characterized in that, described weight percentages of components is: Fructus Hippophae total flavones 45%, plant sterol 55%.
5. a preparation method for compositions described in claim 1～4, comprises the following steps:
(1) prepare Fructus Hippophae total flavones extract;
(2) prepare plant sterol extract;
(3) take Fructus Hippophae total flavones extract and plant sterol extract, add adjuvant, be prepared into various dosage forms;
The preparation method of the Fructus Hippophae extract described in step (1) comprises: get Fructus Hippophae medical material, add ethyl acetate and ethanol, heating and refluxing extraction after being pulverized, obtain extracting solution I, medicinal residues add ethanol, and heating and refluxing extraction obtains extracting solution II, merge extractive liquid, I and II, be condensed into extractum, use dissolve with ethanol extractum, adopt nonpolar or low pole macroporous resin to carry out separation to it, first with water elution, obtain eluent I; Then with ethanol elution 2 times, the volumetric concentration of eluting ethanol is 50%～60% for the first time, and the volumetric concentration of eluting ethanol is 90%～95% for the second time, obtains eluent II, reclaim, and concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract.
6. the preparation method of Chinese medicine composition according to claim 5, it is characterized in that, the described Fructus Hippophae total flavones preparation method of step (1) comprises: get Fructus Hippophae medical material, the ethyl acetate and 70% ethanol that after being pulverized, add volume ratio 1:2, reflux 1 hour, extract 2 times, 1～3 hour for the first time, 1～2 hour for the second time, filtrate merges to obtain extracting solution I, medicinal residues add 70% ethanol, heating and refluxing extraction 2 times, 0.5～1.5 hour for the first time, 0.5～1 hour for the second time, filtrate merges to obtain extracting solution II, merge extractive liquid, I and II, be condensed into extractum, with 50% dissolve with ethanol extractum, adopt nonpolar or low pole macroporous resin to carry out separation to it, first with water elution, obtain eluent I, then with 50%～60% ethanol elution, then with 90%～95% ethanol elution, obtain eluent II, reclaim, concentrating under reduced pressure, dry, obtain Fructus Hippophae total flavones extract.
7. according to the preparation method of the Chinese medicine composition described in claim 5 or 6, it is characterized in that, the ethyl acetate that step (1) is described and the volume ratio of ethanol are 1:2; , the volumetric concentration of eluting ethanol is 60% for the first time; The volumetric concentration of eluting ethanol is 90% for the second time.
8. according to the preparation method of the Chinese medicine composition described in claim 5 or 6, it is characterized in that, the preparation of the steroidal extract that step (2) is described comprises: raw material drying, pulverize, petroleum ether is or/and 56～70 ℃ of reflux, extract, of ethyl acetate heating, extracting solution concentrating under reduced pressure, must be containing the extractum of solute 40～45%; By on gained condensed cream to etc. on the chromatographic column of weight silica gel, first use petroleum ether: ethyl acetate=95:5 as mobile phase, obtain eluent I, then change petroleum ether: ethyl acetate=85:15 as mobile phase, obtain eluent II; Eluent II air-distillation is concentrated, and when being concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystal crude product, reclaims solvent; By crystal crude product petroleum ether: ethyl acetate=85:15 mixed solvent heating for dissolving, filtration, when filtrate has been concentrated to crystallization, tapping, to crystallisation vessel, cools 2 hours, filters to obtain crystalline product;
Described elution flow rate 0.2～2BV/h, preferred, 0.5～1 BV/h.
9. according to the preparation method of the Chinese medicine composition described in claim 5～8, it is characterized in that, the described elution flow rate of step (1) is 1～4BV/h, is preferably 1～2BV/h, more preferably 2BV/h.
10. according to the preparation method of the Chinese medicine composition described in claim 5～9, it is characterized in that macroporous resin AB～8 or X～5 that step (1) is described, more preferably X～5.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107281233A (en) * | 2016-06-13 | 2017-10-24 | 中国科学院西北高原生物研究所 | Protection purposes of the total seabuckthorn flavone to blood vessel endothelium |
| CN108244649A (en) * | 2018-03-20 | 2018-07-06 | 湖南中沙中医科技有限公司 | There is hippophae rhamnoides fruit oil soft capsule for softening blood vessel and preparation method thereof |
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| CN1672712A (en) * | 2004-03-25 | 2005-09-28 | 李安国 | New recipe and prepn process of blood fat reducing medicine |
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| CN1672712A (en) * | 2004-03-25 | 2005-09-28 | 李安国 | New recipe and prepn process of blood fat reducing medicine |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107281233A (en) * | 2016-06-13 | 2017-10-24 | 中国科学院西北高原生物研究所 | Protection purposes of the total seabuckthorn flavone to blood vessel endothelium |
| CN108244649A (en) * | 2018-03-20 | 2018-07-06 | 湖南中沙中医科技有限公司 | There is hippophae rhamnoides fruit oil soft capsule for softening blood vessel and preparation method thereof |
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Application publication date: 20140115 |
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