CN109966328A - Ellagic acid and the extracting method of chebulinic acid and combinations thereof in a kind of myrobalan - Google Patents

Ellagic acid and the extracting method of chebulinic acid and combinations thereof in a kind of myrobalan Download PDF

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CN109966328A
CN109966328A CN201910357486.7A CN201910357486A CN109966328A CN 109966328 A CN109966328 A CN 109966328A CN 201910357486 A CN201910357486 A CN 201910357486A CN 109966328 A CN109966328 A CN 109966328A
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myrobalan
acid
parts
solvent
refluxing extraction
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白吉日木吐
李金柱
张海玉
赖苏雅拉吐
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Inner Mongolia Arshan Pharmaceutical Co ltd
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    • A61K2236/30Extraction of the material
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    • AHUMAN NECESSITIES
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    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
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    • A61K2236/55Liquid-liquid separation; Phase separation

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Abstract

The present invention relates to Chinese medical extract fields, and in particular to ellagic acid and the extracting method of chebulinic acid and combinations thereof in a kind of myrobalan.The following steps are included: pretreatment, myrobalan is pulverized and sieved;By smashed myrobalan's refluxing extraction, then by miillpore filter, solid A and extracting solution A are obtained;Solid A is subjected to refluxing extraction again, then by miillpore filter, obtains solid B and extracting solution B;Mixed extract A and extracting solution B, concentration, by macroporous absorbent resin, solvent elution, crystallizing and drying obtains ellagic acid and chebulinic acid in myrobalan.Extracting method of the invention can targetedly extract ellagic acid and chebulinic acid in myrobalan, and its content purity is higher.The present invention also provides a kind of products for having positive effect for treatment hypertension, hyperlipidemia, while there are also the effects of inflammation-dimishing and eye brightening.

Description

Ellagic acid and the extracting method of chebulinic acid and combinations thereof in a kind of myrobalan
Technical field
The present invention relates to Chinese medical extract fields, and in particular in a kind of myrobalan the extracting method of ellagic acid and chebulinic acid and Its composition.
Background technique
With the rapid development of economy, bigger transformation has occurred in the dietary structure and habit of people, and many people exist While glutton's sumptuous meal, also result in that Energy intaking is excessive, then hypertension, so-called " rich people's disease " that hyperlipidemia is representative one after another and Come.Hypertension, hyperlipidemia are the sources of many diseases, as people's diet high in fat, with high salt adds unreasonable eating habit, Body metabolism is caused to get muddled.High grease will lead to blood lipid raising, and hyperlipemia is cerebral apoplexy, coronary heart disease, myocardial infarction, sudden Dead risk factor.In addition, hyperlipemia is also to promote hyperlipidemia, impaired glucose tolerance, an important risk factor of diabetes. Hyperlipemia can also result in fatty liver, cirrhosis, cholelithiasis, pancreatitis, fundus hemorrhage, blindness, peripheral vascular disease, limping, Hyperuricemia.So the harm of hyperlipidemia must be paid much attention to, positive prevention and conditioning.Easy induction hypertension with high salt, this Sick general onset is slow, and patient's early stage is often asymptomatic, or the only symptoms such as dizziness, headache, palpitaition, tinnitus, and seemingly one The independent disease of kind, as soon as actually cause the important risk factor of the heart, the cerebrovascular and nephropathy, if malpractice Meeting lesion becomes these common hypertension complications such as more serious headstroke, myocardial infarction and renal failure.
General therapeutic " three high " can efficiently control hypertension, hyperlipidemia based on Western medicine.But Western medicine is effectively being adjusted Meanwhile some adverse reactions are often generated, and such as: diuretic depressor major side effects are one low (Diagnostic value), three high (liters Hyperlipidemia, blood glucose, blood uric acid).Drug side-effect, which has become, influences one of long-term continued treatment and major issue of quality of life, Correctly it must recognize and deal carefully with.
In recent years, tcm field has further progress for the research of myrobalan, it is believed that the effective substance wherein extracted Matter ellagic acid and chebulinic acid have good effect for reducing by three height, inflammation-dimishing and eye brightening, heart tonifying.Modern pharmacological studies have shown that scolding Son has the multiple pharmacological effects such as neuroprotection, anti-oxidant, heart tonifying, antibacterial, antitumor, lower hyperlipidemia, hypertension, hyperglycemia.Main chemical compositions have tan The compounds such as matter class, triterpenes, flavonoids.
Application for a patent for invention CN101433563A discloses a kind of effective component of chebula fruit, and preparation process includes following step It is rapid: step 1: using ethyl acetate and alcohol mixture to extract as solvent to myrobalan, step 2: the dregs of a decoction are extracted with ethyl alcohol, are obtained To extracting solution, step 3: extracting solution obtains eluent by column chromatography.Step 4: being obtained with preparative liquid chromatography gradient elution Eluent, mobile phase be water and acetonitrile, collect 48.0-52.0 minutes eluents obtain active principle.The invention also discloses Preparation method, pharmaceutically acceptable preparation and its application in preparation of anti-tumor drugs.By its attached drawing 1 it is found that it is mentioned Component is taken to be at least 6 kinds, type is complicated, prevent active principle is from preferably playing drug effect.
Application for a patent for invention CN108338996A discloses a kind of method for preparing tannin effective constituents in myrobalan, step As follows: by myrobalan's powder dehydrated alcohol ultrasonic extraction, extracting solution is concentrated under reduced pressure into medicinal extract;It is used after medicinal extract is dissolved with suitable quantity of water Large pore resin absorption column chromatographic isolation, successively with pure water, the ethyl alcohol of volume fraction 20%, 40%, 60%, 80%, 90%, 95% Gradient elution is collected 90% alcohol elution, then is separated through silica gel column chromatography, successively with volume ratio 65:1,55:1,45:1, The chloroform-methanol of 35:1,25:1,10:1 elute, and collect 25:1 elution fraction, are concentrated to obtain the final product.The preparation method can be obtained effectively Tannin effective constituents into myrobalan, have anti-oxidant, antibacterial, anti-tumor activity, and the active component that can be used as myrobalan is answered It is prepared for drug.But it is lower according to the constituent content that its technical solution obtains, purity is smaller.
It finds after study, the chebulinic acid and ellagic acid extracted through myrobalan, which carries out compatibility with other Chinese medicine materials, to be made With for treatment hypertension, hyperlipidemia, inflammation-dimishing and eye brightening with very big facilitation
Application for a patent for invention CN107308290A discloses a kind of lowering blood pressure and blood fat, hypoglycemic health care particle tea, institute It includes: 3-15 parts of Radix Angelicae Sinensis, 3-15 parts of Radix Rehmanniae, peach kernel that lowering blood pressure and blood fat, hypoglycemic health care particle tea, which are stated, according to mass fraction 4-20 parts, 3-15 parts of safflower, 2-10 parts of Fructus Aurantii, 2-10 parts of radix paeoniae rubra, 3-15 parts of radix bupleuri, 2-10 parts of Radix Glycyrrhizae, 2-10 parts of campanulaceae, Rhizoma Chuanxiong 2-10 parts, 3-15 parts of radix achyranthis bidentatae, 3-15 parts of olibanum, 3-15 parts of myrrh, 4-20 parts of dried orange peel, 4-20 parts of rhizoma pinellinae praeparata and 8-22 parts of Poria cocos. The present invention according to the proportion made of health care particle tea, three drops are curative for effect, convenient for taking, having no toxic side effect, by promoting blood circulation, Eleminating phlegm and freeing channels, improves deficient five internal organs, and mode that is inside and outside and adjusting improves function of human body, realizes lowering blood pressure and blood fat, hypoglycemic mesh , the health care prevention suitable for general population needs and rehabilitation needs of curing the disease.But after tested, to reducing blood pressure and blood fat curative effect compared with Difference acts on unobvious.
Application for a patent for invention CN108619108A discloses a kind of Shenqi Xinshu capsules application and preparation method thereof, belongs to Medicine technical field.The Shenqi Xinshu capsules, including the following raw material in parts by weight: 60-120 parts of Radix Notoginseng, Radix Salviae Miltiorrhizae 60- 120 parts, 100-200 parts of ganoderma lucidum, 60-120 parts of Pachyrhizua angulatus, 50-100 parts of safflower, 60-120 parts of Rhizoma Chuanxiong, 90-180 parts of dalbergia wood, Cortex Eucommiae 100-200 parts, 100-200 parts of radix cynanchi atrati, 300-600 parts of cactus, 30-60 parts of Radix Glycyrrhizae.Shenqi Xinshu capsules of the present invention are followed certainly So, simple process, low in cost.The imitative national usage decocting system of preparation method, and in production technology, Radix Notoginseng, Radix Salviae Miltiorrhizae, Pachyrhizua angulatus are with powder It is broken into fine powder to be used as medicine, not only remains to full ingredient effective component, but also instead of 60% shaping auxiliary materials, and also there is good drop Pressure, lipid-loweringing, hypoglycemic, antiplatelet aggregative activity, have wide range of applications.But this application effect is more single, disappears for heat-clearing Effect scorching, improving eyesight is not preferable.
Application for a patent for invention CN102599595A discloses a kind of health beverages with effect for reducing blood fat comprising: in Medicine additive and deionized water, wherein the weight percent of the Chinese medicine additive is 10%-20%, the Chinese medicine additive packet Include following component, kuh-seng, pueraria lobata, wilsonii, the fleece-flower root, puncture vine, gynostemma pentaphylla, rhizoma anemarrhenae, safflower, cassia seed, radix scutellariae, Snakegourd Fruit, chicken Blood rattan, Radix Polygalae, Rhizoma Atractylodis Macrocephalae, seaweed, cape jasmine, pipewort, Radix Glycyrrhizae, Herba Cistanches and Semen Cuscutae.Guarantor containing traditional Chinese medicine ingredients of the invention It is good for drink and the health beverages is prepared using the superhigh pressure technique under specified conditions, the superhigh pressure technique under the specified conditions, The effective component in Chinese medicine can be extracted to greatest extent, improve extraction efficiency, have efficiently, quickly, conveniently, automation etc. it is excellent Gesture, health beverages obtained have significant effect to reducing blood lipid, prevent and treat hyperlipidemia well.This application there is also The single disadvantage of effect is only capable for the treatment of hyperlipidemia, does not have positive effect for hypertension, anti-inflammation and sterilization, improving eyesight.
How much currently, the crowd's resistance perplexed by hypertension, hyperlipidemia is all poor, all there is certain inflammation in body, While treating hypertension, hyperlipidemia, treatment body inflammation be can not be ignored.Ellagic acid in myrobalan is effectively extracted there are no a kind of With the method for chebulinic acid, ellagic acid and chebulinic acid in myrobalan can be targetedly extracted, and its content purity is higher.Existing skill Also there are no a kind of products for having positive effect for treatment hypertension, hyperlipidemia for art, while there are also the effects of inflammation-dimishing and eye brightening.
Summary of the invention
In order to solve in the prior art, purification complicated component, the problems such as purity is not high, the present invention provide tan in a kind of myrobalan Spend the extracting method of acid and chebulinic acid, comprising the following steps:
(1) it pre-processes: myrobalan is pulverized and sieved;
(2) it extracts 1: by smashed myrobalan's refluxing extraction, then by miillpore filter, obtaining solid A and extracting solution A;
(3) 2 are extracted: solid A is subjected to refluxing extraction again, then by miillpore filter, obtains solid B and extracting solution B;
(4) separate: mixed extract A and extracting solution B, concentration pass through macroporous absorbent resin, solvent elution, crystallizing and drying Obtain ellagic acid and chebulinic acid in myrobalan.
Further, the step (1), pulverizes and sieves 200-300 mesh.
Further, the step (2), refluxing extraction solvent for use are Methanol-Ethanol-Water solution;By weight, molten Agent: myrobalan=(8-12): 1, methanol: ethyl alcohol: water=5:(5-10): 1.
Further, the step (2), refluxing extraction condition are as follows: reflux temperature is 45-65 DEG C;Return time is 1-3h.
Further, the step (3), refluxing extraction solvent for use are Acetic Acid-Water solution;By weight, it solvent: scolds Son=(5-10): 1, acetic acid: water=(2-5): 1.
Further, the step (3), refluxing extraction condition are as follows: reflux temperature is 65-80 DEG C;Return time is 1-3h.
Further, the step (4), one of macroporous absorbent resin type HPD-100, D-101 or SD-300.
Further, the step (4), solvent are one of alcohol-water or methanol-water;By weight, it elutes Agent: (extracting solution A+ extracting solution B)=(5-11): 1.
Further, the step (4), according to parts by weight, ethyl alcohol: water=(5-8): 1.
Further, the step (4), according to parts by weight, methanol: water=(2-6): 1.
In order to solve, product efficacy in the prior art is single, cannot treat hypertension, hyperlipemia simultaneously and its bring is scorching The problems such as disease, the present invention provide a kind of hypertension and hyperlipemia, inflammation-dimishing and eye brightening composition, consist of the following compositions: safflower, myrobalan, cape jasmine, Ellagic acid and chebulinic acid extract in Radix Glycyrrhizae and above-mentioned myrobalan.
Further, by weight, consist of the following compositions: 5-15 parts of safflower, 5-15 parts of myrobalan, 1-10 parts of cape jasmine, Ellagic acid and 0.01-0.03 parts of chebulinic acid in 1-8 parts of Radix Glycyrrhizae and myrobalan.
Further, by weight, it consists of the following compositions: 9 parts of safflower, 10 parts of myrobalan, 5 parts of cape jasmine, Radix Glycyrrhizae 3 Part, ellagic acid and 0.01 part of chebulinic acid in myrobalan.
Further, by weight, consist of the following compositions: 5 parts of safflower, 5 parts of myrobalan, 2 parts of cape jasmine, 5 parts of Radix Glycyrrhizae, Ellagic acid and 0.02 part of chebulinic acid in myrobalan.
Further, by weight, safflower: Radix Glycyrrhizae=(1-4): 1, myrobalan: cape jasmine=(1-3): 1.
Further, by weight, safflower: Radix Glycyrrhizae=(1-3): 1, myrobalan: cape jasmine=(1.5-2.5): 1.
Further, by weight, safflower: Radix Glycyrrhizae=3:1, myrobalan: cape jasmine=2:1.
Further, by weight, safflower: Radix Glycyrrhizae=1:1, myrobalan: cape jasmine=2.5:1.
The present invention also provides the preparation methods of above-mentioned composition, comprising the following steps: mixes all components, crushed Sieve, sterilizing, obtains composition.
Further, it crushed 60-80 mesh.
Further, 70 meshes be crushed.
Further, comprising the following steps: by 5-15 parts of safflower, 5-15 parts of myrobalan, 1-10 parts of cape jasmine, 1-8 parts of Radix Glycyrrhizae, scold Ellagic acid and 0.01-0.03 parts of chebulinic acid mixing, crushed 60-80 mesh, sterilize, obtain composition in son.
Further, comprising the following steps: by ellagic acid in 9 parts of safflower, 10 parts of myrobalan, 5 parts of cape jasmine, 3 parts of Radix Glycyrrhizae, myrobalan It is mixed with 0.01 part of chebulinic acid, crushed 70 meshes, sterilized, obtain composition.
Further, comprising the following steps: by ellagic acid in 5 parts of safflower, 5 parts of myrobalan, 2 parts of cape jasmine, 5 parts of Radix Glycyrrhizae, myrobalan It is mixed with 0.02 part of chebulinic acid, crushed 70 meshes, sterilized, obtain composition.
The group that extract, above-mentioned composition or the above-mentioned preparation method obtained the present invention also provides said extracted method obtains Close application of the object in preparation health protection tea.
Theoretical basis:
Safflower, alias red blue flower, thorn safflower, composite family, safflower plant, blood circulation, removing blood stasis and acesodyne, help to control through It closes, dysmenorrhea, lochia, chest impediment and cardialgia, stasis of blood, pricking pain in the chest, traumatic injury, sore swell and ache curative curative effect.There is activating microcirculation and removing stasis medicinal, The effect of dissipate wet effect going to swell, avoids pregnant woman from using, and otherwise will cause miscarriage.
The effect of safflower:
1. inhibiting key role: safflower decoction low dose can make toad isolated heart and rabbit heart in vivo slightly excited, make Heartbeat is strong, and amplitude increases;It is large dosage of then have inhibiting effect to heart, make decreased heart rate, myocardial contractive power weakens, cardiac output It reduces.
2. the experimental study of pair coronary blood flow shows: crude extract from carthamus tinctorius L. with water and safflower water soluble mixt-safflower yellow It is known as the effect for increasing coronary blood flow and cardiac muscle nutritional blood flow;And the expansion coronary artery and increase hat of safflower ethanol extract The effect of arteries and veins blood flow is then unobvious or without influence.
3. pair expeirmental myocardial ischemia and the experimental study of myocardial infarction show: causing the experimental heart in rabbit, rat, dog etc. On myocardial ischemia or the animal model of myocardial infarction, safflower and its preparation have different degrees of antagonism.Safflower can make because hanging down Rat caused by body pituitrin or Rabbits With Acute Myocardial Ischemia have obvious protective function;Repeated Brief can be made to block coronary blood Stream causes the degree of anesthetized dog acute myocardial ischemia substantially reduced, range shorter, decreased heart rate, and protects acute myocardial infarction area Edge, area and reduce infarction size and reduce the amplitude raised of marginal zone ECG ST section, so as to improve ischemic myocardium oxygen Supply-demand relationship.
4. safflower finds vasoactive research: as first with the Rockwell liquid containing micro adrenaline or norepinephrine Perfusion blood vessel makes animal myocardium vessel smooth muscle shrink the vascular tone for keeping certain, causes the blood vessels of possible similar people not Logical, state of blood stasis.Cavy hind leg and rabbit ear that safflower can be such that tonicity increases are presented vasorelaxation action, and increase with dosage and Effect is obvious, and safflower can also increase anesthetized dog femoral artery blood flow, but can be allowed to shrink to the normal myocardium vessel of toad and rabbit. Show that safflower expansion blood vessel function is related with the dosage of the functional status of blood vessel and drug.Its mechanism of action may be mainly direct Or partial agonistic alpha-adrenergic receptor effect and distend the blood vessels, and have weaker direct vasoconstriction effect.
5. influence of the safflower to brain edema caused by experimental animal cerebral arterial thrombosis: using Sofflower injection, (1ml is included Crude drug 1g), preoperative 30 minutes ip are carried out to 63 mongolian gerbils and award 10g/kg Sofflower injection, and set up operating comparison Group and sham-operation group observe influence of the safflower to ischemic brain edema, and the monoaminergic transmitters for having studied same brain area contain The variation of amount.As a result prompt safflower mitigates the mechanism of ischemic brain edema, may can influence monoamine mediated neurotransmission in tissue with it The metabolic disorder of matter is related.And further confirm that safflower can reduce incidence of stroke and the death rate really, experimental chest is obstructed The brain tissue for filling in animal has protective effect.
6. antihypertensive effect: safflower decoction, carthamin yellow and other preparations have anesthetized cat or dog different degrees of fast Fast antihypertensive effect, mean blood pressure decline 20 mm Hgs or so, restore after 30 minutes.
7. analgesia and sedation.
8. anti-inflammatory effect.
The effect of myrobalan:
The effect of myrobalan has relieving diarrhea with astringents, astringes the lung to stop cough, fall fire relieving sore-throat.It is usually used in protracted dysentery and diarrhea, hematochezia rectal prolapse, lung Void is breathed with cough, and is coughed long more than, pharyngalgia hoarse voice.
Myrobalan has stronger detoxicating functions, and the endogenous toxication for both having solved the village perverse trend Ju Yuzang chest can also be released because in food The exogenous toxications such as cytotoxic drug poisoning, middle snake bite.Myrobalan's water decoction has the function of very strong anti-gonococcus in vitro.Myrobalan Alcohol extracting thing, which has, reinforces atrial muscle cell contractile function and excitatoty effect.Terminalia chebula can the short Left atria in contracting place Effective refractory period, reduce the maximum drive frequency of Left atria, improve the excitability of Left atria cell.
The effect of cape jasmine:
Cape jasmine alias Yellow Fructus Gardeniae, mountain Cape jasmine, white toad, have the effects that protect liver, cholagogue, decompression, calmness, hemostasis, detumescence.In Doctor's clinic is usually used in treating the diseases such as icteric hepatitis, bruise, hypertension, diabetes.There is health-care effect, cape jasmine is in common Medicine, Gardenia Yellow play the role of similar cape jasmine, there is capable of clearing heat and reducing internal heat, and cool blood cholagogue reduces the effect of cholesterol, have certain health care Function, be it is a kind of integrate coloring, nutrition, multifunctional health natural plant pigment.
The effect of Radix Glycyrrhizae:
Radix Glycyrrhizae, major function is clearing heat and detoxicating, expelling phlegm and arresting coughing, stomach duct and abdomen etc..
1. antiacid: Radix Glycyrrhizae has similar adrenocortical hormones fuction.There is inhibition to gastroxia caused by histamine Effect;And there is antiacid and alleviation gastrointestinal smooth muscle spasm effect.
2. antibechic: licoflavone, extract of licorice root and enoxolone have apparent antitussive effect;Phlegm-dispelling functions are also relatively aobvious It writes, action intensity is glycyrrhizic acid > licoflavone > extract of licorice root.
3. anti-inflammatory antiallergy: there are also anti-inflammatory, anti-allergic effects for Radix Glycyrrhizae, can protect the throat and tunica mucosa tracheae of inflammation.Radix Glycyrrhizae Medicinal extract has the detoxication of similar glucuronic acid with glycyrrhizic acid to certain poisonous substances.
4. the balance intracorporal hormone of women: Radix Glycyrrhizae is commonly used to treat symptom with climacteric and next, because containing in Radix Glycyrrhizae Glycyrrhizin is a kind of compound of similar hormone, it helps to balance the intracorporal hormone-content of women.
5. anti-curing oncoma: hypo acid contained by Radix Glycyrrhizae can block the effect of Induced by Carcinogen tumour growth.
The present invention provides the extracting methods and one kind of ellagic acid in a kind of myrobalan and chebulinic acid with clearing heat and detoxicating, clear Liver improving eyesight, anti-inflammatory, decompression, lipid-loweringing, heart tonifying, trophic nerve cell, the composition promoted longevity and other effects, with the prior art pair Than, the beneficial effects of the present invention are:
1. by selecting suitable extracting solution and counterflow condition, so that being directed to the extraction of ellagic acid in myrobalan and chebulinic acid Property is stronger, and purity is higher.
2. by selecting suitable chromatographic column and eluent, so that extract components type is simple, to ellagic acid in myrobalan It is stronger with the extraction specific aim of chebulinic acid.
3. reasonable traditional Chinese medicinal components compatibility makes product of the present invention have good hypertension and hyperlipemia effect, simultaneously for disappearing Scorching, improving eyesight also has significant effect.
4. effectively raising product by determining the quality proportioning of safflower and Radix Glycyrrhizae, myrobalan and cape jasmine and decompression being dropped The effect of rouge, inflammation-dimishing and eye brightening.
Specific embodiment
The invention will now be further described with reference to specific embodiments, the advantages and features of the present invention will be with description and It is apparent, but these examples are merely exemplary, it is not intended to limit the scope of the present invention in any way.Those skilled in the art Member it should be understood that without departing from the spirit and scope of the invention can details to technical solution of the present invention and form into Row modifications or substitutions, but these modifications and replacement are fallen within the protection scope of the present invention.
Embodiment 1
The extracting method of ellagic acid and chebulinic acid:
(1) it pre-processes: myrobalan be crushed into 200 meshes;
(2) extract 1: by smashed myrobalan's refluxing extraction, refluxing extraction solvent for use is Methanol-Ethanol-Water solution, Middle methanol: ethyl alcohol: water=5:5:1, solvent: myrobalan=8:1 obtains solid A and extracting solution A then by miillpore filter;Reflux Extraction conditions are as follows: reflux temperature is 45 DEG C;Return time is 1h
(3) 2 are extracted: solid A being subjected to refluxing extraction again, refluxing extraction solvent for use is Acetic Acid-Water solution, wherein vinegar Acid: water=2:1, solvent: myrobalan=5:1 obtains solid B and extracting solution B then by miillpore filter;Refluxing extraction condition are as follows: Reflux temperature is 80 DEG C;Return time is 1h.
(4) separate: mixed extract A and extracting solution B, concentration, by HPD-100 macroporous absorbent resin, mass fraction is 83.3% ethanol-water elution, solvent: (extracting solution A+ extracting solution B)=5:1, crystallizing and drying obtain ellagic acid in myrobalan And chebulinic acid.
The preparation of composition:
5 parts of safflower, 5 parts of myrobalan, 2 parts of cape jasmine, 5 parts of Radix Glycyrrhizae, ellagic acid and 0.02 part of chebulinic acid in myrobalan.
All components are mixed, crushed 60 meshes, sterilizing obtains composition.
Embodiment 2
The extracting method of ellagic acid and chebulinic acid:
(1) it pre-processes: myrobalan be crushed into 300 meshes;
(2) extract 1: by smashed myrobalan's refluxing extraction, refluxing extraction solvent for use is Methanol-Ethanol-Water solution, Middle methanol: ethyl alcohol: water=5:10:1, solvent: myrobalan=12:1 obtains solid A and extracting solution A then by miillpore filter;It returns Flow extraction conditions are as follows: reflux temperature is 65 DEG C;Return time is 3h
(3) 2 are extracted: solid A being subjected to refluxing extraction again, refluxing extraction solvent for use is Acetic Acid-Water solution, wherein vinegar Acid: water=5:1, solvent: myrobalan=10:1 obtains solid B and extracting solution B then by miillpore filter;Refluxing extraction condition Are as follows: reflux temperature is 65 DEG C;Return time is 3h.
(4) separate: mixed extract A and extracting solution B, concentration, by SD-300 macroporous absorbent resin, mass fraction is 88.9% ethanol-water elution, solvent: (extracting solution A+ extracting solution B)=11:1, crystallizing and drying obtain ellagic acid in myrobalan And chebulinic acid.
The preparation of composition:
15 parts of composition components safflower, 15 parts of myrobalan, 10 parts of cape jasmine, 8 parts of Radix Glycyrrhizae, ellagic acid and chebulinic acid 0.03 in myrobalan Part.
All components are mixed, crushed 80 meshes, sterilizing obtains composition.
Embodiment 3
The extracting method of ellagic acid and chebulinic acid:
(1) it pre-processes: myrobalan be crushed into 250 meshes;
(2) extract 1: by smashed myrobalan's refluxing extraction, refluxing extraction solvent for use is Methanol-Ethanol-Water solution, Middle methanol: ethyl alcohol: water=5:8:1, solvent: myrobalan=10:1 obtains solid A and extracting solution A then by miillpore filter;It returns Flow extraction conditions are as follows: reflux temperature is 50 DEG C;Return time is 2h
(3) 2 are extracted: solid A being subjected to refluxing extraction again, refluxing extraction solvent for use is Acetic Acid-Water solution, wherein vinegar Acid: water=3:1, solvent: myrobalan=8:1 obtains solid B and extracting solution B then by miillpore filter;Refluxing extraction condition are as follows: Reflux temperature is 70 DEG C;Return time is 2h.
(4) separate: mixed extract A and extracting solution B, concentration, by D-101 macroporous absorbent resin, mass fraction is 66.7% methanol-water solvent elution, solvent: (extracting solution A+ extracting solution B)=8:1, crystallizing and drying obtain ellagic acid in myrobalan And chebulinic acid.
The preparation of composition:
9 parts of safflower, 10 parts of myrobalan, 5 parts of cape jasmine, 3 parts of Radix Glycyrrhizae, ellagic acid and 0.01 part of chebulinic acid in myrobalan.
All components are mixed, crushed 70 meshes, sterilizes, obtains composition.
Embodiment 4
The extracting method of ellagic acid and chebulinic acid:
(1) it pre-processes: myrobalan be crushed into 300 meshes;
(2) extract 1: by smashed myrobalan's refluxing extraction, refluxing extraction solvent for use is Methanol-Ethanol-Water solution, Middle methanol: ethyl alcohol: water=5:7:1, solvent: myrobalan=9:1 obtains solid A and extracting solution A then by miillpore filter;Reflux Extraction conditions are as follows: reflux temperature is 55 DEG C;Return time is 1.5h
(3) 2 are extracted: solid A being subjected to refluxing extraction again, refluxing extraction solvent for use is Acetic Acid-Water solution, wherein vinegar Acid: water=4:1, solvent: myrobalan=7:1 obtains solid B and extracting solution B then by miillpore filter;Refluxing extraction condition are as follows: Reflux temperature is 75 DEG C;Return time is 2.5h.
(4) separate: mixed extract A and extracting solution B, concentration, by D-101 macroporous absorbent resin, mass fraction is 66.7% methanol-water solvent elution, solvent: (extracting solution A+ extracting solution B)=10:1, crystallizing and drying obtain ellagic acid in myrobalan And chebulinic acid.
The preparation of composition:
5 parts of safflower, 5 parts of myrobalan, 1 part of cape jasmine, 1 part of Radix Glycyrrhizae, ellagic acid and 0.01 part of chebulinic acid in myrobalan.
All components are mixed, crushed 70 meshes, sterilizes, obtains composition.
Comparative example 1
Compared with Example 3, composition is different, and compatibility mode is different.
48 parts of kuh-seng, 22 parts of pueraria lobata, 22 parts of wilsonii, 32 parts of the fleece-flower root, 32 parts of puncture vine, 38 parts of gynostemma pentaphylla, 68 parts of rhizoma anemarrhenae, 20 parts of safflower, 16 parts of cassia seed, 32 parts of radix scutellariae, 15 parts of Snakegourd Fruit, 16 parts of Caulis Spatholobi, 11 parts of Radix Polygalae, 32 parts of Rhizoma Atractylodis Macrocephalae, 15 parts of seaweed, 32 parts of cape jasmine, 22 parts of pipewort, 38 parts of Radix Glycyrrhizae, 38 parts of Herba Cistanches and 32 parts of Semen Cuscutae.
All components are mixed, crushed 70 meshes, sterilizes, obtains composition.
Comparative example 2
Compared with Example 3, safflower is different from Radix Glycyrrhizae content, but weight proportion is identical.
18 parts of safflower, 10 parts of myrobalan, 5 parts of cape jasmine, 6 parts of Radix Glycyrrhizae.
All components are mixed, crushed 70 meshes, sterilizes, obtains composition.
Comparative example 3
Compared with Example 3, each component content, proportion are different.
2 parts of safflower, 4 parts of myrobalan, 12 parts of cape jasmine, 9 parts of Radix Glycyrrhizae, ellagic acid and 0.06 part of chebulinic acid in myrobalan.
All components are mixed, crushed 70 meshes, sterilizes, obtains composition.
Comparative example 4
Compared with Example 3, extraction process, that is, step (2-3) is different in the extracting method of ellagic acid and chebulinic acid.
Wherein, (2) extract 1: by smashed myrobalan's refluxing extraction, refluxing extraction solvent for use is ethanol-water solution, Middle ethyl alcohol: water=8:1, solvent: myrobalan=10:1 obtains solid A and extracting solution A then by miillpore filter;Refluxing extraction item Part are as follows: reflux temperature is 75 DEG C;Return time is 1h
(3) 2 are extracted: solid A being subjected to refluxing extraction again, refluxing extraction solvent for use is methanol-water solution, wherein first Alcohol: water=3:1, solvent: myrobalan=8:1 obtains solid B and extracting solution B then by miillpore filter;Refluxing extraction condition are as follows: Reflux temperature is 4 DEG C;Return time is 2h.
Comparative example 5
Compared with Example 3, separation process, that is, step (4) is different in the extracting method of ellagic acid and chebulinic acid.
Wherein, (4) separate: mixed extract A and extracting solution B, concentration, pass through DM130 type macroporous absorbent resin, quality point Number elutes for 80% ethanol-water, solvent: (extracting solution A+ extracting solution B)=4:1, and crystallizing and drying obtains tan flower in myrobalan Acid and chebulinic acid.
1 assay of effect example
Using the content of high effective liquid chromatography for measuring ellagic acid and chebulinic acid.Chromatographic column be C18 (4.6mm × 250mm, 5 μm);Mobile phase is the methanol-water that volume fraction is 50%;Flow velocity 1mL/min.
Test result see the table below:
Group Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Comparative example 4 Comparative example 5
Ellagic acid purity 52.3% 51.6% 53.1% 52.7% 36.8% 40.1%
Chebulinic acid purity 45.3% 44.6% 45.6% 44.9% 32.6% 36.4%
2 fat-reducing effect of effect example
Male SD rat 80,150 ± 10g of weight are taken, is randomly divided into 8 groups, every group 10, feeds high lipid food to knot is administered Beam claims respectively wherein 4 groups start simultaneously at tea beverage made of the composition of stomach-filling embodiment 1-4 preparation in feeding high lipid food For embodiment 1-4 group;3 groups start simultaneously at tea beverage made of the composition of stomach-filling comparative example 1-3 preparation in feeding high lipid food, It is referred to as comparative example 1-3 group;1 group starts simultaneously at stomach-filling water in feeding high lipid food, and referred to as high in fat group;Stomach-filling capacity presses 1mL/ 10g batheroom scale, every group is administered 30 days altogether.
Tea beverage made of tea beverage made of the composition of embodiment 1-4 preparation and the composition of comparative example 1-3 preparation Preparation method: take 10g composition, 100ml80 DEG C of water be added, impregnate 10min, be cooled to room temperature.
High lipid food composition are as follows: 80% basal feed, 10% lard, 9.5% yolk powder and 0.5% Pig cholate.
After last day fasting for 24 hours is administered, rat femoral takes blood, and centrifuging and taking serum measurement TC (total cholesterol), TG are (sweet Oily three esters), HDL-C (high-density lipoprotein cholesterol), experimental result see the table below.
Note: the same test item, P < 0.05 between different letters.
3 antihypertensive effect of effect example
Spontaneous hypertension rat 70,150 ± 10g of weight are taken, is randomly divided into 7 groups, every group 10, wherein 4 groups in feeding Feed starts simultaneously at tea beverage made of the composition of stomach-filling embodiment 1-4 preparation, is referred to as embodiment 1-4 group;3 groups are being fed Food feed starts simultaneously at tea beverage made of the composition of stomach-filling comparative example 1-3 preparation, is referred to as comparative example 1-3 group;In addition 10 normal rats start simultaneously at stomach-filling water as a control group, in feeding feed.Stomach-filling capacity presses 1.0mL/10g batheroom scale, even It is 30 days continuous.
Tea beverage made of tea beverage made of the composition of embodiment 1-4 preparation and the composition of comparative example 1-3 preparation Preparation method: take 10g composition, 100ml80 DEG C of water be added, impregnate 10min, be cooled to room temperature.
Animal adaptability is raised after a week, detects the systolic pressure of groups of animals, diastole respectively with noninvasive arteria caudalis blood pressure instrument Pressure.After gastric infusion, These parameters are detected again.Experimental result see the table below:
Note: the same test item, P < 0.05 between different letters.
4 anti-inflammatory effect of effect example
The detection of CRP is widely used in monitoring different inflammatory conditions, it can also be used to monitor the therapeutic effect to inflammation.
Taking rat 70 with inflammation, 150 ± 10g of weight is randomly divided into 7 groups, and every group 10, wherein 4 groups in feeding Feed starts simultaneously at tea beverage made of the composition of stomach-filling embodiment 1-4 preparation, is referred to as embodiment 1-4 group;3 groups are being fed Food feed starts simultaneously at tea beverage made of the composition of stomach-filling comparative example 1-3 preparation, is referred to as comparative example 1-3 group;In addition 10 normal rats start simultaneously at stomach-filling water as a control group, in feeding feed.Stomach-filling capacity presses 1.0mL/10g batheroom scale, even It is 30 days continuous.
Tea beverage made of tea beverage made of the composition of embodiment 1-4 preparation and the composition of comparative example 1-3 preparation Preparation method: take 10g composition, 100ml80 DEG C of water be added, impregnate 10min, be cooled to room temperature.
Animal adaptability is raised after a week, and rat femoral takes blood, and centrifuging and taking serum measures the content of CRP in serum, gives After medicine last day fasting for 24 hours, rat femoral takes blood, and centrifuging and taking serum measures the content of CRP in serum.Experimental result is seen below Table:
Group Raise CRP (mg/L) after a week CRP (mg/L) after administration
Control group 8.6±1.2a 7.2±2.1c
Embodiment 1 21.4±1.6a 12.1±1.4b
Embodiment 2 22.6±1.5a 10.3±1.5b
Embodiment 3 20.9±1.7a 9.8±2.2b
Embodiment 4 21.8±2.1a 8.5±1.7b
Comparative example 1 22.1±1.9a 20.3±1.8b
Comparative example 2 20.5±2.2a 16.6±1.4b
Comparative example 3 21.8±1.9a 14.8±2.1b
Note: P < 0.05 between different letters.
Integration test result is it is found that the application has following advantages:
1. by selecting suitable extracting solution and counterflow condition, so that being directed to the extraction of ellagic acid in myrobalan and chebulinic acid Property is stronger, and purity is higher.
2. by selecting suitable chromatographic column and eluent, so that extract components type is simple, to ellagic acid in myrobalan It is stronger with the extraction specific aim of chebulinic acid.
3. reasonable traditional Chinese medicinal components compatibility makes product of the present invention have good anti-inflammatory, decompression, fat-reducing effect, while right Also there is significant effect in improving eyesight.
4. effectively raising product by determining the quality proportioning of safflower and Radix Glycyrrhizae, myrobalan and cape jasmine and decompression being dropped The effect of rouge, inflammation-dimishing and eye brightening.
The technical means disclosed in the embodiments of the present invention is not limited only to above-mentioned disclosed technological means, further includes by the above skill Technical solution composed by art feature any combination.The foregoing is a specific embodiment of the present invention, it is noted that for this For the those of ordinary skill of technical field, without departing from the principle of the present invention, it can also make several improvements and repair Decorations, these also will be regarded as protection scope of the present invention.

Claims (10)

1. the extracting method of ellagic acid and chebulinic acid in a kind of myrobalan, which comprises the following steps:
(1) it pre-processes: myrobalan is pulverized and sieved;
(2) it extracts 1: by smashed myrobalan's refluxing extraction, then by miillpore filter, obtaining solid A and extracting solution A;
(3) 2 are extracted: solid A is subjected to refluxing extraction again, then by miillpore filter, obtains solid B and extracting solution B;
(4) separate: mixed extract A and extracting solution B, concentration, by macroporous absorbent resin, solvent elution, crystallizing and drying is obtained Ellagic acid and chebulinic acid in myrobalan.
2. extracting method according to claim 1, which is characterized in that the step (1) pulverizes and sieves 200-300 mesh.
3. extracting method according to claim 1, which is characterized in that the step (2), refluxing extraction solvent for use are first Alcohol-ethanol-water solution;By weight, solvent: myrobalan=(8-12): 1, methanol: ethyl alcohol: water=5:(5-10): 1.
4. extracting method according to claim 1, which is characterized in that the step (2), refluxing extraction condition are as follows: reflux Temperature is 45-65 DEG C;Return time is 1-3h.
5. extracting method according to claim 1, which is characterized in that the step (3), refluxing extraction solvent for use are vinegar Acid-aqueous solution;By weight, solvent: myrobalan=(5-10): 1, acetic acid: water=(2-5): 1.
6. extracting method according to claim 1, which is characterized in that the step (3), refluxing extraction condition are as follows: reflux Temperature is 65-80 DEG C;Return time is 1-3h.
7. extracting method according to claim 1, which is characterized in that the step (4), macroporous absorbent resin type are One of HPD-100, D-101 or SD-300.
8. extracting method according to claim 1, which is characterized in that the step (4), solvent are alcohol-water or methanol- One of water;By weight, solvent: (extracting solution A+ extracting solution B)=(5-11): 1.
9. a kind of hypertension and hyperlipemia, inflammation-dimishing and eye brightening composition, which is characterized in that include any extraction side claim 1-8 The ellagic acid and chebulinic acid that method obtains.
10. the preparation method of composition as claimed in claim 9, which comprises the following steps: mix all components It closes, pulverizes and sieves, sterilize, obtain composition.
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