CN105998248A - Frostbite liniment containing Changbai mountain prunus tomentosa - Google Patents

Frostbite liniment containing Changbai mountain prunus tomentosa Download PDF

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CN105998248A
CN105998248A CN201610329995.5A CN201610329995A CN105998248A CN 105998248 A CN105998248 A CN 105998248A CN 201610329995 A CN201610329995 A CN 201610329995A CN 105998248 A CN105998248 A CN 105998248A
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nanking cherry
liniment
compositions
freeze proof
cherry
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CN105998248B (en
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张成义
陈曦
赵南晰
李贺
陈建光
孙晶波
王曼丽
王明科
熊蔚蔚
郭菁
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Beihua University
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/73Rosaceae (Rose family), e.g. strawberry, chokeberry, blackberry, pear or firethorn
    • A61K36/736Prunus, e.g. plum, cherry, peach, apricot or almond
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/70Web, sheet or filament bases ; Films; Fibres of the matrix type containing drug
    • A61K9/7015Drug-containing film-forming compositions, e.g. spray-on

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Abstract

The invention discloses frostbite liniment containing prunus tomentosa. The frostbite liniment contains prunus tomentosa frostbite-resistant composition. During using, the frostbite liniment is applied to the affected part, a thin film is formed to protect the wound surface, the treatment function is realized through sustained release, breathability, skin adhesion performance and moisture retention performance of the frostbite liniment are better than those of a traditional dosage form such as an adhesive plaster and the like, and the frostbite liniment has the advantages of being comfortable to use, low in skin irritation, convenient to strip and re-paste and the like and is a novel ideal transdermal absorption preparation for external use.

Description

Changbai Mountain Nanking cherry cold injury liniment
Technical field
The present invention relates to field of pharmaceutical preparations, be specifically related to a kind of Changbai Mountain Nanking cherry cold injury liniment.
Background technology
Cold injury (chilblain) is the frequently-occurring disease of cold district or cold season, the degree of damage and cold intensity, humidity, wind Speed, endure cold time and state locally or systemically, body constitution has direct relation, is mainly in hands, foot, face etc. acral Or exposure portion cold injury.This disease is mainly in north refrigerant latitudes, recently as the deterioration of earth environment, the many of south China Area occurs the case of cold injury (chilblain) to increase the most year by year at December to February, and especially army's training or people are in the winter time Carrying out open air to do industry cold injury the most often occurs, as treatment is easy to ulceration not in time, at diabrosis, delay difficulty is more, more after recurrent relatively By force, having seriously undermined the fighting capacity of army and reduced the work efficiency of people, the most serious compromises the healthy of people, freezes The preventing and treating of wound is the important topic of military field all the time, is also the very important problem of civil health.
At present, treat cold injury many uses steroidal anti-inflammatory drugs, nonsteroidal antiinflammatory drug, antithrombotic both at home and abroad and improve micro- Circulation medicine etc. is treated, and motherland's medical science is damaged with warming the meridian, cold relieving dredging collateral, promoting the circulation of blood blood stasis dispelling, softening tissue, improves that body surface is micro-to follow Ring, improving human body resisting cold ability is that base therapy principle is treated.But the most unsatisfactory, steroid, nonsteroidal antiinflammatory drug It is used for multiple times and can produce various untoward reaction, after repeatedly Reusability may occur in which atrophoderma, pigmentation, tolerance and drug withdrawal Easily recur;Antithrombotic and improve microcirculation medicine and need whole body to apply, repeatedly Reusability may occur in which hemorrhage, and to freezing The inflammatory reaction unrestraint effect of wound, is likely to result in Secondary cases pathogenic infection, especially chemical drugs dosage and is difficult to control, consumption Too small drug effect is the best, the excessive untoward reaction that there will be again drug induccd of consumption;Existing treatment by Chinese herbs medicine majority uses and invigorates blood circulation Blood stasis dispelling medicine and phytohormone class medicine, and majority is compound recipe, and research and use are brought inconvenience.
Among the people spread the most always Nanking cherry steep in wine treatment cold injury proved recipe, in recent years this seminar pass through great many of experiments industry Have proven to the freeze proof wound effect of Nanking cherry, and primarily determine that the effective site of freeze proof wound in Fructus Pruni pseudocerasi.
Fructus Pruni pseudocerasi (cherry) is Rosaceae (Rosacesa) Prunus (Prunus L) perennial woody plant, in originating from State, has the cultivation history of more than 2000, China various places all to have cultivation.Especially the Changbai Mountain area distribution with northeast is more.Fructus Pruni pseudocerasi Sarcocarp is delicious and tasty, has beauty functions, also the effect of Dietotherapy health.Nanking cherry primary growth is in Jilin Province, due to weather The factors such as soil, its characteristic unique, conventional wine soaking therapy cold injury among the people.
Cherry pulp currently receives significant attention and studies, and especially attaches most importance to anthocyanin class material, abroad to Anthocyanin from Blueberry Class material carried out extract research, find that it has good antioxidation, also there are some researches prove its have protection cardiovascular and cerebrovascular vessel and Anti-inflammatory activity.
Fructus Pruni pseudocerasi treatment cold injury of steeping in wine is notable by extensive application among the people and effect, takes red deeper fresh Fructus Pruni pseudocerasi number piece, depending on Depending on area is put in painting on the skin, rotten with hand rubbing, enucleation extracting juice, it is coated with and puts on the skin in place of the winter gets chilblains, rub simultaneously and dry, washing away after 24h, The over one hundred example of anti-treating chilblain, evident in efficacy and be difficult to recurrence.The ethanol of fresh Fructus Pruni pseudocerasi immersion 80% soaks 7 days, smears at cold injury, right Can effect a radical cure from the beginning of cold injury.
The pharmacological research of Fructus Pruni pseudocerasi treatment cold injury is shown in " Changbai Mountain Nanking cherry total flavones is on cold injury and inflammation associated impact " (" China Immunology Journal ", 2010, volume 26,11 phases, Zhang Chengyi, Shao Shihe, Shi Yuling), " Nanking cherry ethanol extraction Experimental study " (" Chinese experimental pharmacology of Chinese medical formulae magazine, ", 2010,16 (10), Sun Jingbo, Xu Jing, Chen Lu, Li Yan, Zhang Chengyi) " Deng in literary composition.
External preparation development difficulty is big, Beihua University have submitted 201110455480.7, discloses a kind of cold injury for the treatment of The ointment of ethanol extraction Nanking cherry flavonoid.
But, ointment belongs to traditional external preparation, and the external preparation developed in recent years also only has spray, aerosol Agent, cataplasma, patch, novel form phoenix feathers and unicorn horns, market share is the most limited.According to the feedback of patient, these dosage forms Medicine major part also exist to varying degrees drug loading too low, stimulate skin, can not pathological changes local the long period stop, Onset is slow, use the shortcoming such as inconvenience, contamination medicated clothing.
Liniment is the novel form that development in recent years is got up, and is applied to affected part during use, forms thin film to protect after solvent volatilization Protecting wound surface, the most gradually release contained drug plays therapeutical effect.Its breathability, the most excellent to skin tackness, moisture retention In traditional dosage form rubber-emplastrum etc., there is use comfortable, little to skin irritation, and peel off, paste the advantages such as convenient again, simultaneously The formation of film decreases the evaporation of skin surface moisture, promotes hydration and dissolves cutin effect, making medicine pass through cutin Gradually discharge medicine, add that the use (azone, DMSO etc.) of modern Percutaneous absorption enhancer can make effective ingredient preferably Through Cutaneous permeation to damage location, onset time can be shortened, extend duration of efficacy, be that a kind of preferably Novel external is saturating Skin absorbable preparation.
Therefore, exploitation low toxicity is efficient, and easy to use freeze proof hinders external new drug novel formulation Nanking cherry cold injury film Agent will have great importance.
Summary of the invention
The freeze proof liniment hindering compositions of Nanking cherry, it is characterised in that contain: Nanking cherry is freeze proof hinders compositions;A kind of or many Plant pharmaceutically acceptable carrier such as: substrate, stabilizer, emulsifying agent increases the stability of said composition.
Nanking cherry is freeze proof hinders compositions, it is characterised in that: by Fructus Pruni pseudocerasi petroleum ether part and Nanking cherry macroporous resin position group Become.
Nanking cherry is freeze proof hinders compositions, it is characterised in that: by Fructus Pruni pseudocerasi petroleum ether part 1-10 weight portion and Nanking cherry macropore Resin position 200-500 weight portion composition.
The preparation method of Fructus Pruni pseudocerasi petroleum ether part is: Nanking cherry ethanol extraction, reclaim ethanol, extractum add water make molten, add Petroleum ether, petroleum ether and aqueous solution extraction, merge petroleum ether layer, reclaims petroleum ether and obtains Nanking cherry petroleum ether part;
The preparation method at Nanking cherry macroporous resin position is: Nanking cherry ethanol extraction, reclaim ethanol, extractum add water make molten, Add petroleum ether, petroleum ether and aqueous solution extraction, combining water layer, be dried, cross macroporous resin with ethanol, reclaim ethanol and obtain Nanking cherry Macroporous resin position;
The preparation method at Nanking cherry macroporous resin position is: macroporous adsorbent resin is middle polarity, low pole or nonpolar suction Attached resin, such as D101, HPD100, AB-8, HPD400, HPD600 etc., concentration of alcohol scope is 70%-90% ethanol, loading stream Speed is 1-3BV/h, elution flow rate 1-2BV/h, and eluant volume is 1-8 times of column volume.
Nanking cherry is freeze proof hinders compositions, it is characterised in that: containing one or more pharmaceutically acceptable carrier such as substrate, surely Determining agent, emulsifying agent increases the stability of said composition.
Nanking cherry is freeze proof hinders compositions, it is characterised in that: said composition makes liniment.
The freeze proof liniment hindering compositions of Nanking cherry
Nanking cherry is freeze proof hinders compositions, by Nanking cherry petroleum ether part 1-10mg and Nanking cherry macroporous resin position 200- 500mg forms.
Nanking cherry is freeze proof, and to hinder compositions liniment formulated by following component:
Nanking cherry is freeze proof hinders compositions, by Nanking cherry petroleum ether part 0.5-5mg and Nanking cherry macroporous resin position 100- 500mg forms.
Nanking cherry is freeze proof, and to hinder compositions liniment formulated by following component:
Nanking cherry is freeze proof hinders compositions, by Nanking cherry petroleum ether part 0.5-5mg and Nanking cherry macroporous resin position 100- 500mg forms.
Nanking cherry is freeze proof hinders compositions liniment, it is characterised in that described filmogen also includes hypromellose, hydroxyl Propyl cellulose, polyvinyl alcohol, Lac, xanthan gum, arabic gum, tragacanth, carrageenin, guar gum, elsinan, Pu Lu One in orchid, agar or combination in any.
Nanking cherry is freeze proof hinders compositions liniment, it is characterised in that described plasticizer is selected from Polyethylene Glycol, glycerol, glycerol One or more in one acid esters, diglyceride, propylene glycol, Polysorbate.
Nanking cherry is freeze proof hinders compositions liniment, it is characterised in that described absorption enhancer selected from benzalkonium chloride, azone, A kind of or the most multiple in Polysorbate, sodium lauryl sulphate;
Nanking cherry is freeze proof hinders compositions liniment, it is characterised in that also include polyoxyethylene sorbitan monoleate, polysorbate 60, poly-mountain One in pear ester 20 or combination in any.
Nanking cherry is freeze proof hinders compositions liniment, it is characterised in that other adjuvants described can comprise antioxidant, anticorrosion Agent, antioxidant one in butylated hydroxyanisole, butylated hydroxytoluene, disodium edetate, vitamin C, sodium sulfite, sodium pyrosulfite Or multiple, preservative material can be selected from one or more in sodium benzoate, potassium sorbate, methyl hydroxybenzoate, ethyl hydroxybenzoate.
The freeze proof compositions liniment of hindering of Nanking cherry, the thickness of described liniment is 20 μm~50 μm.
The freeze proof preparation technology hindering compositions liniment of Nanking cherry:
First benzalkonium chloride or azone, glycerol and polyoxyethylene sorbitan monoleate are joined in aqueous solution, after stirring and dissolving, add hydroxyl hydroxyl The filmogen such as propyl cellulose or xanthan gum, is sufficiently stirred for dissolving and obtains glue, adds that Nanking cherry is freeze proof hinders compositions also Stirring, to being uniformly dispersed, obtains the freeze proof compositions glue of hindering of Nanking cherry, stirs deaeration under vacuum, by pastille glue after deaeration Liquid scraper is spread evenly across on polyester belt, 70~80 DEG C of heat dryings, cuts into certain size, obtains Nanking cherry freeze proof wound combination Thing liniment.
The present invention has the advantage that with good effect:
Liniment is the novel form that development in recent years is got up, and is applied to affected part during use, forms thin film to protect after solvent volatilization Protecting wound surface, the most gradually release contained drug plays therapeutical effect.Its breathability, the most excellent to skin tackness, moisture retention In traditional dosage form rubber-emplastrum etc., there is use comfortable, little to skin irritation, and peel off, paste the advantages such as convenient again, simultaneously The formation of film decreases the evaporation of skin surface moisture, promotes hydration and dissolves cutin effect, making medicine pass through cutin Gradually discharge medicine, add that the use (azone, DMSO etc.) of modern Percutaneous absorption enhancer can make effective ingredient preferably Through Cutaneous permeation to damage location, onset time can be shortened, extend duration of efficacy, be that a kind of preferably Novel external is saturating Skin absorbable preparation.Therefore, the freeze proof external new drug novel formulation Nanking cherry cold injury of hindering that exploitation low toxicity is efficient and easy to use is coated with Membrane will have great importance.
Below in conjunction with specific embodiment, the invention will be further described, but does not limit protection scope of the present invention.
Detailed description of the invention
Embodiment 1
Nanking cherry is freeze proof, and to hinder compositions liniment formulated by following component:
Nanking cherry is freeze proof hinders compositions, by Nanking cherry petroleum ether part 1mg and the Nanking cherry macroporous resin portion of embodiment 10 Position 200mg composition
First benzalkonium chloride, glycerol and polyoxyethylene sorbitan monoleate are joined in aqueous solution, after stirring and dissolving, add hydroxyl hydroxypropyl fine Dimension element, be sufficiently stirred for dissolving and obtain hydroxypropyl cellulose blank glue, add Nanking cherry freeze proof hinder compositions and stir to divide Dissipate uniformly, obtain the freeze proof compositions glue of hindering of Nanking cherry, stir deaeration under vacuum, by pastille glue scraper after deaeration It is spread evenly across on polyester belt, 70~80 DEG C of heat dryings, cuts into certain size, obtain that Nanking cherry is freeze proof hinders compositions film Agent.
Embodiment 2
Nanking cherry is freeze proof, and to hinder compositions liniment formulated by following component:
Nanking cherry is freeze proof hinders compositions, by Nanking cherry petroleum ether part 10mg and the Nanking cherry macroporous resin portion of embodiment 10 Position 500mg composition
First azone, glycerol and polyoxyethylene sorbitan monoleate are joined in aqueous solution, after stirring and dissolving, add hydroxyl hydroxy propyl cellulose Element, is sufficiently stirred for dissolving and obtains hydroxypropyl cellulose glue, add Nanking cherry freeze proof hinder compositions and stir to being uniformly dispersed, Obtain the freeze proof compositions glue of hindering of Nanking cherry, stir deaeration under vacuum, pastille glue scraper after deaeration is uniformly coated with It is distributed on polyester belt, 70~80 DEG C of heat dryings, cuts into certain size, obtain that Nanking cherry is freeze proof hinders compositions liniment.
Embodiment 3
Nanking cherry is freeze proof, and to hinder compositions liniment formulated by following component:
Nanking cherry is freeze proof hinders compositions, by Nanking cherry petroleum ether part 1mg and the Nanking cherry macroporous resin portion of embodiment 10 Position 200mg composition
First azone, benzalkonium chloride, glycerol and polyoxyethylene sorbitan monoleate are joined in aqueous solution, after stirring and dissolving, add hydroxyl hydroxyl Propyl cellulose, is sufficiently stirred for dissolving and obtains glue, add Nanking cherry freeze proof hinder compositions and stir to being uniformly dispersed, obtain The freeze proof compositions glue of hindering of Nanking cherry, stirs deaeration under vacuum, is spread evenly across by pastille glue scraper after deaeration On polyester belt, 70~80 DEG C of heat dryings, cut into certain size, obtain that Nanking cherry is freeze proof hinders compositions liniment.
Embodiment 4
Nanking cherry is freeze proof, and to hinder compositions liniment formulated by following component:
Nanking cherry is freeze proof hinders compositions, by Nanking cherry petroleum ether part 10mg and the Nanking cherry macroporous resin portion of embodiment 10 Position 500mg composition
First azone, glycerol and polyoxyethylene sorbitan monoleate are joined in aqueous solution, add ethanol in proper amount, after stirring and dissolving, add Gelatin, is sufficiently stirred for dissolving and obtains gelatin glue, add Nanking cherry freeze proof hinder compositions and stir to being uniformly dispersed, obtain hair The freeze proof compositions glue of hindering of Fructus Pruni pseudocerasi, stirs deaeration under vacuum, is spread evenly across poly-by pastille glue scraper after deaeration On ester band, 70~80 DEG C of heat dryings, cut into certain size, obtain that Nanking cherry is freeze proof hinders compositions liniment.
Embodiment 5
Nanking cherry is freeze proof, and to hinder compositions liniment formulated by following component:
Nanking cherry is freeze proof hinders compositions, by Nanking cherry petroleum ether part 10mg and the Nanking cherry macroporous resin portion of embodiment 10 Position 500mg composition.
First azone, glycerol and polyoxyethylene sorbitan monoleate are joined in aqueous solution, after stirring and dissolving, add xanthan gum, fully stir Mix dissolving and obtain glue, add Nanking cherry freeze proof hinder compositions and stir to being uniformly dispersed, obtain Nanking cherry freeze proof wound combination Composition glue liquid, stirs deaeration under vacuum, is spread evenly across on polyester belt by pastille glue scraper after deaeration, 70~80 DEG C Heat drying, cuts into certain size, obtains that Nanking cherry is freeze proof hinders compositions liniment.
Embodiment 6
Nanking cherry is freeze proof, and to hinder compositions liniment formulated by following component:
First benzalkonium chloride, glycerol and polyoxyethylene sorbitan monoleate are joined in aqueous solution, add ethanol in proper amount, after stirring and dissolving, Add xanthan gum, be sufficiently stirred for dissolving and obtain xanthan gum glue, add Nanking cherry macroporous resin position and stir to dispersion all Even, obtain the glue at Nanking cherry macroporous resin position, stir deaeration under vacuum, by equal for pastille glue scraper after deaeration Even coat on polyester belt, 70~80 DEG C of heat dryings, cut into certain size, obtain that Nanking cherry is freeze proof hinders compositions liniment.
Embodiment 7
Nanking cherry is freeze proof, and to hinder compositions liniment formulated by following component:
First azone, xanthan gum and polyoxyethylene sorbitan monoleate are joined in aqueous solution, add ethanol in proper amount, after stirring and dissolving, add Enter gelatin, be sufficiently stirred for dissolving and obtain glue, add Nanking cherry petroleum ether part and stir to being uniformly dispersed, obtaining Nanking cherry The glue of petroleum ether part, stirs deaeration under vacuum, and pastille glue scraper after deaeration is spread evenly across polyester belt On, 70~80 DEG C of heat dryings, cut into certain size, obtain that Nanking cherry is freeze proof hinders compositions liniment.
Embodiment 8
In order to measure the preparation stability from embodiment 1-6, membrane is put into the aluminum pipe of closing, then at 40 ± 1 DEG C, 75 ± 5%RH (relative humidity) is placed 6 months.Flavones content, flavones content is detected by the HPLC method of embodiment 14 Fall is 0.59%, and this shows that the stability of preparation of embodiment 1-6 is high.
The observation of embodiment 9 Drug therapy of the present invention chilblain
For verifying the therapeutic effect of the present invention, taking 80 rabbits, with the rabbit ear cold injury modeling of two, left and right, left ear is administered, with the right side Ear does own control, does not give any medicine, and stochastic averagina is divided into 8 groups,
Positive drug control group: give sodium heparin vitamin E emulsifiable paste according to 500mg/ kilogram,
Embodiment 1-7 group: give liniment according to 500mg/ kilogram,
First day, with detection congestion and edema area,
After four days, the area of detection congestion and edema,
Calculating inhibitory rate of intumesce is as follows.
Positive drug control group: 40.7%
Embodiment 1:68.4%
Embodiment 2:63.2%
Embodiment 3:64.1%
Embodiment 5:70.3%
Embodiment 6:42.1%
Embodiment 7:71.6%;
Use the product of the present invention, find no any untoward reaction.
Being administered the 7th day, embodiment 1-7 group, treatment ear congestion and edema disappears substantially, and treatment ear compares with compareing ear, swelling Degree has significant difference (p < 0.001), and product of the present invention is light to the rabbit ear, moderate cold injury has significant therapeutic effect.
Being administered the 7th day, histopathology is visible:
Positive drug control group: under light microscopic, visible a large amount of neutrophilic granulocytes ooze out, and erythrocyte infiltrates, tissue looseness's edema,
Embodiment 1-7 group: under treatment otoscope, neutrophilic granulocyte oozes out on a small quantity, inorganization edema;
It is administered the 7th day, by rabbit ear cold injury tissue homogenate detection PGE2 is shown, compares with model control group, positive drug The suppression ratio of thing matched group is 46.8%: the average inhibition of embodiment 1-5 group is 61.9%, and the suppression ratio of embodiment 6 is 31.2%, the suppression ratio of embodiment 7 is 66.7%.
It is administered the 7th day, by rabbit ear Virus monitory MDA is shown, compares with model group, pressing down of positive drug control group Rate processed is 39.2%: the average inhibition of embodiment 1-5 group is 57.6%, and the suppression ratio of embodiment 6 is 45.1%, embodiment 7 Suppression ratio be 59.2%.
It is administered the 7th day, by rabbit ear Virus monitory SOD is shown, compares with model group, carrying of positive drug control group High percent is 11.6%: the average percentage rate that improves of embodiment 1-5 group is 47.5%, and the raising percentage rate of embodiment 6 is 24.3%, the raising percentage rate of embodiment 7 is 47.6%.
It is administered the 7th day, by rabbit ear Virus monitory NO is shown, compares with model group, the suppression of positive drug control group Rate is 21.7%: the average inhibition of embodiment 1-5 group is 39.2%, and the suppression ratio of embodiment 6 is 26.3%, embodiment 7 Suppression ratio is 35.6%.
Embodiment 10
The preparation method of Fructus Pruni pseudocerasi petroleum ether part is: Nanking cherry 10 times amount ethanol extraction 3 times, 1h/ time, merges ethanol and carries Taking liquid, reclaim ethanol, extractum adds suitable quantity of water to be made molten, adds petroleum ether, petroleum ether and aqueous solution and extracts three times according to 1:1, merges Petroleum ether layer, reclaims petroleum ether, vacuum drying, obtains Nanking cherry petroleum ether part;
The preparation method at Nanking cherry macroporous resin position is: Nanking cherry 10 times amount ethanol extraction 3 times, 1h/ time, merges second Alcohol extract, reclaims ethanol, and extractum adds suitable quantity of water to be made molten, adds petroleum ether, petroleum ether and aqueous solution and extracts three times according to 1:1, Combining water layer, is dried, Nanking cherry water extract dry powder water is made into 1mg/mL solution, according to the loading of 1.0g powder/mL resin Amount low pole macroporous resin D-101 adsorbs, and loading flow velocity is (0.3 times column volume/hour), after resin fully adsorbs, first uses Water elution, to without alpha-Naphthol positive reaction, then carries out eluting with 5 times of column volume 80% ethanol, and (elution flow rate is 0.8 times of cylinder Long-pending/hour), collect the eluent of 80% ethanol, be concentrated into without alcohol, vacuum drying, obtain Nanking cherry 80% ethanol macroporous resin portion Position.
Embodiment 11
The preparation method of Fructus Pruni pseudocerasi petroleum ether part is: Nanking cherry 10 times amount ethanol extraction 3 times, 1h/ time, merges ethanol and carries Taking liquid, reclaim ethanol, extractum adds suitable quantity of water to be made molten, adds petroleum ether, petroleum ether and aqueous solution and extracts three times according to 1:1, merges Petroleum ether layer, reclaims petroleum ether, vacuum drying, obtains Nanking cherry petroleum ether part;
The preparation method at Nanking cherry macroporous resin position is: Nanking cherry 10 times amount ethanol extraction 3 times, 1h/ time, merges second Alcohol extract, reclaims ethanol, and extractum adds suitable quantity of water to be made molten, adds petroleum ether, petroleum ether and aqueous solution and extracts three times according to 1:1, Combining water layer, is dried, Nanking cherry water extract dry powder water is made into 1mg/mL solution, according to the loading of 1.0g powder/mL resin Amount low pole macroporous resin D-101 adsorbs, and loading flow velocity is (0.3 times column volume/hour), after resin fully adsorbs, first uses Water elution, to without alpha-Naphthol positive reaction, then carries out eluting with 5 times of column volume 70% ethanol, and (elution flow rate is 0.8 times of cylinder Long-pending/hour), collect the eluent of 70% ethanol, be concentrated into without alcohol, vacuum drying, obtain Nanking cherry 70% ethanol macroporous resin portion Position.
The screening scheme of embodiment 12 extraction process
The preparation method of Fructus Pruni pseudocerasi petroleum ether part is: Nanking cherry 10 times amount water extraction 3 times, 1h/ time, merges water extraction Liquid, adds petroleum ether, petroleum ether and aqueous extract and extracts three times according to 1:1, merge petroleum ether layer, reclaim petroleum ether, and vacuum is done Dry, obtain Nanking cherry petroleum ether part;
The preparation method at Nanking cherry macroporous resin position is: Nanking cherry 10 times amount water extraction 3 times, 1h/ time, merges water and carries Take liquid, add petroleum ether, petroleum ether and aqueous extract and extract three times according to 1:1, combining water layer, it is dried, by Nanking cherry water extract Dry powder water is made into 1mg/mL solution, adsorbs with low pole macroporous resin D-101 according to the applied sample amount of 1.0g powder/mL resin, Loading flow velocity is (0.3 times column volume/hour), after resin fully adsorbs, first washes with water to without alpha-Naphthol positive reaction, then Eluting is carried out with 5 times of column volume 80% ethanol, (elution flow rate be 0.8 times of column volume/hour), collect the eluting of 80% ethanol Liquid, is concentrated into without alcohol, vacuum drying, obtains Nanking cherry 80% ethanol macroporous resin position.
The screening scheme of embodiment 13 extraction process
The preparation method of Fructus Pruni pseudocerasi petroleum ether part is: Nanking cherry 10 times amount water extraction 3 times, 1h/ time, merges water extraction Liquid, adds petroleum ether, petroleum ether and aqueous extract and extracts three times according to 1:1, merge petroleum ether layer, reclaim petroleum ether, and vacuum is done Dry, obtain Nanking cherry petroleum ether part;
The preparation method at Nanking cherry macroporous resin position is: Nanking cherry 10 times amount water extraction 3 times, 1h/ time, merges water and carries Take liquid, add petroleum ether, petroleum ether and aqueous extract and extract three times according to 1:1, combining water layer, it is dried, by Nanking cherry water extract Dry powder water is made into 1mg/mL solution, adsorbs with low pole macroporous resin D-101 according to the applied sample amount of 1.0g powder/mL resin, Loading flow velocity is (0.3 times column volume/hour), after resin fully adsorbs, first washes with water to without alpha-Naphthol positive reaction, then Eluting is carried out with 5 times of column volume 70% ethanol, (elution flow rate be 0.8 times of column volume/hour), collect the eluting of 70% ethanol Liquid, is concentrated into without alcohol, vacuum drying, obtains Nanking cherry 70% ethanol macroporous resin position.
The HPLC of embodiment 14 Nanking cherry flavone analyzes method:
Chromatographic column is Agilent Zorbax Extend-C18 post (2.1mm × 150mm, 5m).Detection wavelength 360nm, post Temperature 25 DEG C, flow velocity 0.5mL/min, acetonitrile-0.85% acetic acid water (20-80 volume ratio) isocratic elution, with Quercetin as reference substance.
Embodiment 10 Nanking cherry macroporous resin position, is 77.8% total flavones containing weight content, and main peak occurs in 17.1min Quercetin.
Embodiment 11 Nanking cherry macroporous resin position, is 66.3% total flavones containing weight content, and main peak occurs in 18.5min Quercetin.
Embodiment 12 Nanking cherry macroporous resin position, is 62.7% total flavones containing weight content, and main peak occurs in 19.3min Quercetin.
Embodiment 13 Nanking cherry macroporous resin position, is 61.9% total flavones containing weight content, and main peak occurs in 18.7min Quercetin.

Claims (4)

1. the freeze proof liniment hindering compositions of Nanking cherry, it is characterised in that:
Compositions is hindered containing Nanking cherry is freeze proof;
Containing one or more pharmaceutically acceptable carrier such as substrate, stabilizer, emulsifying agent increases the stability of said composition.
The freeze proof liniment hindering compositions of Nanking cherry the most according to claim 1, it is characterised in that:
Nanking cherry is freeze proof hinders compositions 1g-5g
Filmogen 30g-90g
Plasticizer 2g-15g
Absorption enhancer 1g-25g
Other adjuvants 1g-25g.
The freeze proof liniment hindering compositions of Nanking cherry the most according to claim 1, it is characterised in that:
Formulated by following component:
Nanking cherry is freeze proof hinders compositions, by Nanking cherry petroleum ether part 0.5-5mg and Nanking cherry macroporous resin position 100-500mg Composition.
The freeze proof membrane hindering compositions of Nanking cherry the most according to claim 1, it is characterised in that:
Formulated by following component:
Nanking cherry is freeze proof hinders compositions, by Nanking cherry petroleum ether part 0.5-5mg and Nanking cherry macroporous resin position 100-500mg Composition.
CN201610329995.5A 2016-05-17 2016-05-17 Changbai Mountain Nanking cherry frostbite plastics Expired - Fee Related CN105998248B (en)

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CN103181961A (en) * 2011-12-30 2013-07-03 北华大学 Preparation method of flavonoid medicine for treating frostbite

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