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CN105727104A - Medicine composition with effects of diminishing inflammation and relieving cough and method for preparing medicine composition - Google Patents

Medicine composition with effects of diminishing inflammation and relieving cough and method for preparing medicine composition Download PDF

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Publication number
CN105727104A
CN105727104A CN201610135695.3A CN201610135695A CN105727104A CN 105727104 A CN105727104 A CN 105727104A CN 201610135695 A CN201610135695 A CN 201610135695A CN 105727104 A CN105727104 A CN 105727104A
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Prior art keywords
acid
medicine composition
pharmaceutical composition
resin
extraction
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韦艳红
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GUANGXI TIANTIANLE PHARMACEUTICAL CO Ltd
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GUANGXI TIANTIANLE PHARMACEUTICAL CO Ltd
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Priority to CN201610135695.3A priority Critical patent/CN105727104A/en
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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)
    • A61K36/88Liliopsida (monocotyledons)
    • A61K36/904Stemonaceae (Stemona family), e.g. croomia
    • 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
    • A61K36/06Fungi, e.g. yeasts
    • A61K36/07Basidiomycota, e.g. Cryptococcus
    • A61K36/076Poria
    • AHUMAN NECESSITIES
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    • 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)
    • A61K36/27Asclepiadaceae (Milkweed family), e.g. hoya
    • AHUMAN NECESSITIES
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    • 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)
    • A61K36/48Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
    • A61K36/484Glycyrrhiza (licorice)
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    • A61K36/57Magnoliaceae (Magnolia family)
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    • 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
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    • A61K36/75Rutaceae (Rue family)
    • A61K36/752Citrus, e.g. lime, orange or lemon
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    • 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)
    • A61K36/79Schisandraceae (Schisandra family)
    • AHUMAN NECESSITIES
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    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/88Liliopsida (monocotyledons)
    • A61K36/888Araceae (Arum family), e.g. caladium, calla lily or skunk cabbage
    • A61K36/8888Pinellia
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/26Carbohydrates, e.g. sugar alcohols, amino sugars, nucleic acids, mono-, di- or oligo-saccharides; Derivatives thereof, e.g. polysorbates, sorbitan fatty acid esters or glycyrrhizin
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    • A61K9/0087Galenical forms not covered by A61K9/02 - A61K9/7023
    • A61K9/0095Drinks; Beverages; Syrups; Compositions for reconstitution thereof, e.g. powders or tablets to be dispersed in a glass of water; Veterinary drenches
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    • A61K9/16Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605Excipients; Inactive ingredients
    • A61K9/1629Organic macromolecular compounds
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    • A61K2236/30Extraction of the material
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    • A61K2236/331Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
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Abstract

The invention relates to a medicine composition with effects of diminishing inflammation and relieving cough and a method for preparing the medicine composition. The medicine composition comprises, by weight, exocarpium citri grandis, radix stemonae, poria, rhizoma pinelliae, rhizoma cynanchi stauntonii, radix glycyrrhizae, semen armeniacae amarum and fructus schisandrae chinensis. The method for preparing the medicine composition includes distilling the exocarpium citri grandis and the semen armeniacae amarum by the aid of steam; extracting the radix glycyrrhizae and the rhizoma pinelliae by the aid of ethyl alcohol and then extracting the radix glycyrrhizae and the rhizoma pinelliae by the aid of organic solvents; extracting the honey-processed radix stemonae, the honey-processed poria, the honey-processed rhizoma cynanchi stauntonii and the honey-processed fructus schisandrae chinensis by the aid of water; combining extract to obtain the medicine composition. The medicine composition and the method have the advantages that effects of regulating qi-flowing for eliminating phlegm and moistening lungs for relieving the cough can be realized by the medicine composition, and the medicine composition is applicable to the cough, asthma and excessive phlegm due to turbid phlegm obstructing lungs; as observed clinically, definite curative effects are realized by the medicine composition for common cold, bronchitis and faucitis, and toxic and side effects are unfound.

Description

A kind of pharmaceutical composition of inflammation-diminishing and cough-controlling and preparation method thereof
Technical field
The present invention relates to tcm field, be specifically related to pharmaceutical composition of a kind of inflammation-diminishing and cough-controlling and preparation method thereof.
Background technology
Expectorant is turbid stays in lung, and be jammed air flue, clinical with cough with asthma, uncomfortable in chest, abundant expectoration rale be main manifestations card.Be common in cough, breathe heavily, roar, pulmonary distension, lung abscess, and the disease such as the bronchitis of doctor trained in Western medicine, pneumonia.The origin cause of formation of turbid phlegm obstructing in the lung has inside and outside two kinds: endogenous cause of ill is relevant with spleen, as excessive in eating and drinking without temperance, overstrain impairing the spleen, or seven emotions, insufficiency of the spleen mistake all can be made to transport, it is impossible to ascending the clear and descending the turbid, stop gathering with bringing about the spread of body fluid, become expectorant turbid, upper general in lung, therefore have saying of " spleen being the source rising expectorant, the lung being the utensil for storing phlegm ".Exopathogenic factor is then violated lung by wind, heat, the pathogen such as dry, or wind and cold enters inner heat-transformation, and bright liquid becomes expectorant, forms expectorant heat and stops up and hinder in lung;Or the heresy of affection of exogenous wind-cold, send out in priming phlegm retention, become obstruction of the lung by cold-phlegm.
Juhong Tanke liquid is 2010 editions first disclosed compound recipes of the Pharmacopoeia of the People's Republic of China, the preparation method disclosing prescription composition and tablet, capsule.Disclosed extracting method is as follows:
Exocarpium Citri Grandis, the Radix Stemonae, Poria, the Rhizoma Pinelliae, Rhizoma Cynanchi Stauntonii, Radix Glycyrrhizae, Semen Armeniacae Amarum, Fructus Schisandrae Chinensis etc. eight taste, Exocarpium Citri Grandis, Semen Armeniacae Amarum vapor distillation, collect distillate 80ml, the Six-elements such as medicinal residues and all the other Radixs Stemonae, boiling secondary, each 2 hours, collecting decoction, filter, it is the clear paste of 1.25-1.35 that filtrate is concentrated into relative density when 80 DEG C, adding ethanol makes alcohol content be 75%-80%, stand 24 hours, take supernatant, reclaim ethanol and to be concentrated into relative density when 80 DEG C be the clear paste of 1.18-1.20, with sucrose 400g, Mel 100g, sodium benzoate 3g, ethyl hydroxybenzoate 0.3g, it is stirred to dissolve, add above-mentioned distillate, mixing, filter, let cool, add essence and Mentholum is appropriate, add water to 1000ml, stir evenly, obtain.
Owing to the character of Chinese crude drug active component is different, as adopted said method first Exocarpium Citri Grandis, Semen Armeniacae Amarum vapor distillation, medicinal residues the whole water extract-alcohol precipitation of all the other medical materials, last united extraction liquid makes oral liquid, owing to effective ingredient is without extracting completely, in use medicine fails to play whole effect, thus affecting drug effect.
Accordingly, it is desirable to provide a kind of active component extraction ratio that can improve medicine, with the preparation method improving pharmaceutical effectiveness.
Summary of the invention
It is an object of the invention to provide a kind of pharmaceutical composition for inflammation-diminishing and cough-controlling.
The preparation method that it is an object of the invention to provide a kind of pharmaceutical composition for inflammation-diminishing and cough-controlling.
Pharmaceutical composition for inflammation-diminishing and cough-controlling provided by the invention is made up of the composition of following weight portion: Exocarpium Citri Grandis 300 parts, the processed with honey Radix Stemonae 30 parts, 30 parts of Poria, Rhizoma Pinelliae Preparata 30 parts, Rhizoma Cynanchi Stauntonii 50 parts, 10 parts of Radix Glycyrrhizae, Semen Armeniacae Amarum 100 parts, Fructus Schisandrae Chinensis 20 parts, it is characterized in that, this pharmaceutical composition is prepared from by following methods:
1) Exocarpium Citri Grandis, Semen Armeniacae Amarum vapor distillation, collect distillate, medicinal residues add ethanol extraction, extracting solution crosses neutral alumina, collects effluent, and effluent crosses cationic resin, wash post with water, discard water lotion, use 40%-90% ethanol elution, collecting eluent, resin anion (R.A.) crossed by eluent, washes post with water, discard water lotion, use 40%-90% ethanol elution, collect eluent, concentration, obtains extract A;
2) extracting liquorice, the Rhizoma Pinelliae add ethanol extraction, and extracting solution filters, and filtrate adds the mixing of 3-10% alkali liquor, stands, and filters, discarding precipitation, filtrate adds organic solvent extraction, collects aqueous alkali layer, and pH to 3-4 is adjusted in acid to add 2%, add organic solvent extraction, collect organic solvent layer, reclaim organic solvent, obtain extract B;
3) taking the processed with honey Radix Stemonae, after Poria, Rhizoma Cynanchi Stauntonii, Fructus Schisandrae Chinensis soak, boil extraction, extracting solution filters, and filtrate concentrates, and obtains extract C;
4) united extraction thing A, B, C, dry, to obtain final product.
Preferably, described step 1) in alkali liquor be: in sodium hydroxide, potassium carbonate, potassium bicarbonate, sodium carbonate, sodium bicarbonate, sodium citrate, potassium citrate, sodium sesquicarbonate, sodium dihydrogen citrate one or more.
Preferably, described step 1) in acid be: in citric acid, lactic acid, phosphoric acid, tartaric acid, malic acid, metatartaric acid, acetic acid, hydrochloric acid, adipic acid, fumaric acid one or more.
Preferably, described step 1) cationic resin is: in 732 strongly acidic styrene type cation exchange resins, 734 strongly acidic styrene type cation exchange resins, D254 macroporous strong basic quaternary ammonium cation exchanger resin, D-61 large hole strong acid styrene system cation exchange resin one or more.
Preferably, described step 1) in resin anion (R.A.) be: in 717 strong-basicity styrene series anion exchange resins, 711 strong-basicity styrene series I type anion exchange resin, D311 macroporous acrylic system weak basic anion exchange resin, D318 macroporous acrylic system weak acid anion exchanger resin one or more.
Preferably, described step 2) in organic solvent be: in ethyl acetate, chloroform, normal butane, dichloromethane or ether one or more.
The preparation method that the invention provides aforementioned pharmaceutical compositions, specifically includes following steps:
1) Exocarpium Citri Grandis, Semen Armeniacae Amarum vapor distillation, collect distillate, medicinal residues add 8-10 times of medical material weight 50%-80% alcohol reflux 1-3 time, each 1-3 hour, united extraction liquid, extracting solution crosses neutral alumina, collect effluent, effluent crosses cationic resin, with the washing post of 2 times of weight resins, discard water lotion, continue with 2 times of weight resin 40%-90% ethanol elutions, collect eluent, eluent continued resin anion (R.A.), with the washing post of 2 times of weight resins, discard water lotion, continue with 2 times of weight resin 40%-90% ethanol elutions, collect eluent, being concentrated into relative density when 60-80 DEG C is 1.1-1.2, obtain extract A;
2) extracting liquorice, Rhizoma Pinelliae 40%-90% alcohol heating reflux extract 1-3 time, the every time ethanol of addition medical material weight 6-10 times, each extraction time is 1-3 hour, filtering, merging filtrate, filtrate adds the sodium carbonate that concentration is 3-10%, stand, filter, discard precipitation, filtrate adds chloroform and extracts 3 times, collects aqueous alkali layer, and the hydrochloric acid that aqueous alkali layer adds 2% adjusts pH to 3-4, chloroform extracts, collect chloroform layer, reclaim chloroform, obtain extract B;
3) take the honey Radix Stemonae, Poria, Rhizoma Cynanchi Stauntonii, Fructus Schisandrae Chinensis added the water soaking of medical material weight 6-10 times after 60 minutes, boiled extraction 1-3 time, and each 1-3 hour, united extraction liquid, filtration, it was 1.1-1.2 that filtrate is concentrated into relative density when 60-80 DEG C, obtains extract C;
4) united extraction thing A, B, C, vacuum drying, to obtain final product.
Present invention also offers the preparation containing aforementioned pharmaceutical compositions, said preparation is separately made by pharmaceutical composition or is made up of pharmaceutical composition and pharmaceutically acceptable carrier.
Present invention also offers the application in the medicine preparing inflammation-diminishing and cough-controlling of aforementioned pharmaceutical compositions or preparation.
Chinese medicine composition of the present invention is detected by inventor, find to use technical solution of the present invention to prepare gained Chinese medicine composition naringin, amygdaloside, glycyrrhizic acid, Rhizoma Pinelliae total acid content significantly high, compared with existing extraction process products obtained therefrom, both have notable difference, and testing result indicates the extraction of some effective ingredient in each component from the side and is better than prior art.Owing to every taste Chinese crude drug all contains many active component, at least not yet there is any a herb purely and simply to be analyzed and know all the components, different Chinese medicine combines when extracting with different extracting modes, due to influencing each other and acting between solvent, temperature and heterogeneity, extremely complex chemical reaction can be produced.Therefore, above-mentioned effective ingredient is a part for Chinese medicine extract active component, and the drug action impact for overall medicine is still not clear.We contrast different extracting mode quality in certain therapeutic use only by effect experiment at present, and the method that there is no changes from the change indicator of part effective ingredient to the curative effect judging compound Chinese patent medicine.Therefore, we observe, by actual animal pharmacodynamics test, the change that drug effect occurs after process reform, and the results show, sample prepared by technical solution of the present invention is really better than prior art and prepares sample.
One provided by the invention is treated colpitic pharmaceutical composition and is had the advantage that
1, the embodiment sample naringin prepared by technical solution of the present invention, amygdaloside, glycyrrhizic acid, Rhizoma Pinelliae total acid content are all remarkably higher than comparative example, experimental result prompting adopts naringin, amygdaloside, glycyrrhizic acid, Rhizoma Pinelliae total acid in the technology of the present invention extraction gained Chinese medicine composition compared with prior art, to extract more complete.
2, results of pharmacodynamic test shows: the embodiment sample prepared by technical solution of the present invention can extend mouse cough incubation period, reduces cough number of times in 3min, points out extractive technique scheme of the present invention to be better than prior art, it is possible to significantly improve the curative effect effect of antitussive.
3, not finding untoward reaction in clinical trial, safety detection, efficacy test do not find and test relevant new abnormal case.
Detailed description of the invention
Following example are used for illustrating the present invention, but are not limited to the scope of the present invention.
If no special instructions, the concentration of alcohol in the present invention is percent by volume.
Embodiment 1: scheme one is extracted
1) raw material is weighed by following deal: Exocarpium Citri Grandis 3kg, processed with honey Radix Stemonae 0.3kg, Poria 0.3kg, Rhizoma Pinelliae Preparata 0.3kg, Rhizoma Cynanchi Stauntonii 0.5kg, Radix Glycyrrhizae 0.1kg, Semen Armeniacae Amarum 1kg, Fructus Schisandrae Chinensis 0.2kg.
2) Exocarpium Citri Grandis, Semen Armeniacae Amarum vapor distillation, collect distillate, medicinal residues add 10 times of medical material weight 50% alcohol reflux 1 time, extract 3 hours, filter, extracting solution crosses neutral alumina, collect effluent, effluent crosses 732 cationic resin, with the washing post of 2 times of weight resins, discard water lotion, continue with 2 times of weight resin 40% ethanol elutions, collect eluent, eluent continued 717 resin anion (R.A.)s, with the washing post of 2 times of weight resins, discard water lotion, continue with 2 times of weight resin 40% ethanol elutions, collect eluent, being concentrated into relative density when 60 DEG C is 1.1, obtain extract A;
3) extracting liquorice, the Rhizoma Pinelliae 40% alcohol heating reflux extract 1 time, add medical material weight 10 times ethanol, extraction time is 3 hours, filtering, filtrate adds the sodium carbonate that concentration is 3%, stands, filtering, discard precipitation, filtrate adds chloroform and extracts 3 times, collect aqueous alkali layer, the hydrochloric acid that aqueous alkali layer adds 2% adjusts pH to 3.0, and chloroform extracts, and collects chloroform layer, reclaim chloroform, obtain extract B;
4) take the honey Radix Stemonae, Poria, Rhizoma Cynanchi Stauntonii, Fructus Schisandrae Chinensis added the water soaking of medical material weight 10 times after 60 minutes, boiled extraction 1 time, 3 hours, filtered, and it is 1.1 that filtrate is concentrated into relative density when 60-80 DEG C, obtains extract C;
4) united extraction thing A, B, C, vacuum drying, pulverize, add appropriate starch, carboxymethyl cellulose, microcrystalline Cellulose, granulate, dry, granulate, tabletting, coating, obtain tablet.
Embodiment 2:
1) raw material is weighed by following deal: Exocarpium Citri Grandis 3kg, processed with honey Radix Stemonae 0.3kg, Poria 0.3kg, Rhizoma Pinelliae Preparata 0.3kg, Rhizoma Cynanchi Stauntonii 0.5kg, Radix Glycyrrhizae 0.1kg, Semen Armeniacae Amarum 1kg, Fructus Schisandrae Chinensis 0.2kg.
2) Exocarpium Citri Grandis, Semen Armeniacae Amarum vapor distillation, collect distillate, medicinal residues add 8-10 times of medical material weight 60% alcohol reflux 2 times, each 2 hours, united extraction liquid, extracting solution crosses neutral alumina, collect effluent, effluent crosses 734 cationic resin, with the washing post of 2 times of weight resins, discard water lotion, continue with 2 times of weight resin 60% ethanol elutions, collect eluent, eluent continued 711 resin anion (R.A.)s, with the washing post of 2 times of weight resins, discard water lotion, continue with 2 times of weight resin 60% ethanol elutions, collect eluent, being concentrated into relative density when 70 DEG C is 1.15, obtain extract A;
3) extracting liquorice, the Rhizoma Pinelliae 60% alcohol heating reflux extract 2 times, add the ethanol of medical material weight 8 times every time, each extraction time is 2 hours, filtering, merging filtrate, filtrate adds the sodium bicarbonate that concentration is 5%, stand, filter, discard precipitation, filtrate adds diethyl ether and extracts 3 times, collects aqueous alkali layer, and the citric acid that aqueous alkali layer adds 2% adjusts pH to 3.5, ether extracts, collect chloroform layer, reclaim chloroform, obtain extract B;
4) take the honey Radix Stemonae, Poria, Rhizoma Cynanchi Stauntonii, Fructus Schisandrae Chinensis added the water soaking of medical material weight 8 times after 60 minutes, boiled extraction 2 times, each 2 hours, and united extraction liquid filters, and it is 1.15 that filtrate is concentrated into relative density when 70 DEG C, obtains extract C;
5) united extraction thing A, B, C, vacuum drying, pulverize, add appropriate starch, granulate, dry, granulate, encapsulated, obtain capsule.
Embodiment 3:
1) raw material is weighed by following deal: Exocarpium Citri Grandis 3kg, processed with honey Radix Stemonae 0.3kg, Poria 0.3kg, Rhizoma Pinelliae Preparata 0.3kg, Rhizoma Cynanchi Stauntonii 0.5kg, Radix Glycyrrhizae 0.1kg, Semen Armeniacae Amarum 1kg, Fructus Schisandrae Chinensis 0.2kg.
2) Exocarpium Citri Grandis, Semen Armeniacae Amarum vapor distillation, collect distillate, medicinal residues add 8-10 times of medical material weight 75% alcohol reflux 3 times, extract 1 hour every time, united extraction liquid, extracting solution crosses neutral alumina, collect effluent, effluent crosses D254 cationic resin, with the washing post of 2 times of weight resins, discard water lotion, continue with 2 times of weight resin 75% ethanol elutions, collect eluent, eluent continued D311 resin anion (R.A.), with the washing post of 2 times of weight resins, discard water lotion, continue with 2 times of weight resin 80% ethanol elutions, collect eluent, being concentrated into relative density when 75 DEG C is 1.2, obtain extract A;
3) extracting liquorice, the Rhizoma Pinelliae 80% alcohol heating reflux extract 3 times, add the ethanol of medical material weight 10 times every time, each extraction time is 1 hour, filtering, merging filtrate, filtrate adds the sodium carbonate that concentration is 8%, stand, filter, discard precipitation, filtrate adds extraction into ethyl acetate 3 times, collects aqueous alkali layer, and pH to 3.8 adjusted by the fumaric acid that aqueous alkali layer adds 2%, extraction into ethyl acetate, collect ethyl acetate layer, reclaim ethyl acetate, obtain extract B;
4) take the honey Radix Stemonae, Poria, Rhizoma Cynanchi Stauntonii, Fructus Schisandrae Chinensis added the water soaking of medical material weight 10 times after 60 minutes, boiled extraction 3 times, each 1 hour, and united extraction liquid filters, and it is 1.2 that filtrate is concentrated into relative density when 75 DEG C, obtains extract C;
5) united extraction thing A, B, C, vacuum drying, pulverize, add appropriate starch, granulate, dry, granulate, subpackage, obtain granule.
Embodiment 4:
1) raw material is weighed by following deal: Exocarpium Citri Grandis 3kg, processed with honey Radix Stemonae 0.3kg, Poria 0.3kg, Rhizoma Pinelliae Preparata 0.3kg, Rhizoma Cynanchi Stauntonii 0.5kg, Radix Glycyrrhizae 0.1kg, Semen Armeniacae Amarum 1kg, Fructus Schisandrae Chinensis 0.2kg.
2) Exocarpium Citri Grandis, Semen Armeniacae Amarum vapor distillation, collect distillate, medicinal residues add 10 times of medical material weight 90% alcohol reflux 3 times, extract 1 hour every time, united extraction liquid, extracting solution crosses neutral alumina, collect effluent, effluent crosses D-61 cationic resin, with the washing post of 2 times of weight resins, discard water lotion, continue with 2 times of weight resin 95% ethanol elutions, collect eluent, eluent continued D318 resin anion (R.A.), with the washing post of 2 times of weight resins, discard water lotion, continue with 2 times of weight resin 90% ethanol elutions, collect eluent, being concentrated into relative density when 80 DEG C is 1.2, obtain extract A;
3) extracting liquorice, the Rhizoma Pinelliae 90% alcohol heating reflux extract 3 times, add the ethanol of medical material weight 10 times every time, each extraction time is 1 hour, filtering, merging filtrate, filtrate adds the sodium carbonate that concentration is 10%, stand, filter, discard precipitation, filtrate adds extraction into ethyl acetate 3 times, collects aqueous alkali layer, and pH to 4.0 adjusted by the fumaric acid that aqueous alkali layer adds 2%, extraction into ethyl acetate, collect ethyl acetate layer, reclaim ethyl acetate, obtain extract B;
4) take the honey Radix Stemonae, Poria, Rhizoma Cynanchi Stauntonii, Fructus Schisandrae Chinensis added the water soaking of medical material weight 10 times after 60 minutes, boiled extraction 3 times, each 1 hour, and united extraction liquid filters, and it is 1.2 that filtrate is concentrated into relative density when 80 DEG C, obtains extract C;
5) united extraction thing A, B, C, mixing, add appropriate sucrose, purified water, potassium sorbate, fill, obtain oral liquid.
Comparative example 1:
Raw material is weighed: Exocarpium Citri Grandis 3kg, processed with honey Radix Stemonae 0.3kg, Poria 0.3kg, Rhizoma Pinelliae Preparata 0.3kg, Rhizoma Cynanchi Stauntonii 0.5kg, Radix Glycyrrhizae 0.1kg, Semen Armeniacae Amarum 1kg, Fructus Schisandrae Chinensis 0.2kg by following deal.
Above eight tastes, Exocarpium Citri Grandis, Semen Armeniacae Amarum vapor distillation, collect distillate 80ml, the Six-elements such as medicinal residues and all the other Radixs Stemonae, boiling secondary, each 2 hours, collecting decoction, filter, it is the clear paste of 1.25-1.35 that filtrate is concentrated into relative density when 80 DEG C, adding ethanol makes alcohol content be 75%-80%, stand 24 hours, take supernatant, reclaim ethanol and to be concentrated into relative density when 80 DEG C be the clear paste of 1.18-1.20, with sucrose 400g, Mel 100g, sodium benzoate 3g, ethyl hydroxybenzoate 0.3g, it is stirred to dissolve, add above-mentioned distillate, mixing, filter, let cool, add essence and Mentholum is appropriate, add water to 1000ml, stir evenly, obtain.
Experimental example 1: the comparison that different preparation method gained sample sizes measure
1 sample packet
Embodiment 4, comparative example 1.
2 contrast projects
Naringin, amygdaloside, glycyrrhizic acid, Rhizoma Pinelliae total acid content.
3 experimental results, in Table 1
The different preparation method gained sample size measurement result of table 1
Table 1 result shows: embodiment of the present invention sample naringin, amygdaloside, glycyrrhizic acid, Rhizoma Pinelliae total acid content are all remarkably higher than comparative example.Experimental result prompting adopts naringin, amygdaloside, glycyrrhizic acid, Rhizoma Pinelliae total acid in the technology of the present invention extraction gained Chinese medicine composition compared with prior art, to extract more complete.
Pharmacodynamics test
Ammonia is caused the impact of mouse cough
1 material
1.1 laboratory animal cleaning grade Male Kunming strain mice 50, weight 18~22g, Guangxi Medical University's animal center provide.Feeding environment: room temperature 20 23 DEG C, relative humidity 45%~6o%, cage tool peracetic acid soln is sterilized, and drinking water is scrubbing water.
1.2 medicines and reagent
Embodiment 1, embodiment 2, embodiment 3, embodiment 4, comparative example 1;Ammonia (analytical pure).
2 methods
2.1 packets take Male Kunming strain mice 6O only with administration, are randomly divided into 6 groups, only often organize each 1O, often organize and give following medicine respectively by 0.2ml/10g gastric infusion, every day 1 time, continuous 7d:
Blank group: isometric(al) pure water
Embodiment 1, embodiment 2, embodiment 3, embodiment 4, comparative example 1: be all equivalent to crude drug amount 4g/kg, be equivalent to 8 times of adult's quantity.
30min after 2.2 operation last administrations, is placed in each group of mice in inverted 500mL beaker respectively, inside puts a cotton balls, drawing ammonia with 1mL syringe, 0.2mL injects in cotton balls, is inverted rapidly beaker, in order to avoid gas leakage, observe and record cough number of times in mouse cough incubation period and 3min.
3 results are respectively organized cough number of times in mouse cough incubation period and 3min and are compared in Table 1.
Table 1 is respectively organized cough number of times in mouse cough incubation period and 3min and is compared (x ± s)
Note: compare with blank group, * P < 0.05, * * P < 0.01;Compare with comparative example 1 group, #P < 0.05.
From table 1, embodiment 1-4 and 1 group of comparative example compared with blank group, all can extend mouse cough incubation period (P < 0.05, P < 0.01), reduce cough number of times (P < 0.05, P < 0.01) in 3min;But embodiment 1-4 group significance simultaneously is better than comparative example 1 group.Point out extractive technique scheme of the present invention to be better than prior art, the curative effect effect of antitussive can be significantly improved.
4 conclusions
The present invention is Chinese medicine preparation, has activating QI to eliminate phlegm, effect of nourishing the lung to arrest cough, it is adaptable to the cough caused by turbid phlegm obstructing in the lung, asthma, abundant expectoration;Flu, bronchitis, pharyngolaryngitis, by clinical observation determined curative effect, non-invention toxicity, is a kind of new Chinese medicine being worthy to be popularized.And preparation method of the present invention is compared with prior art, curative effect has significant difference.
Although, above use generality explanation, detailed description of the invention and test, the present invention is described in detail, but on basis of the present invention, it is possible to it is made some modifications or improvements, and this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to the scope of protection of present invention.

Claims (8)

1. the pharmaceutical composition of an inflammation-diminishing and cough-controlling, it is made up of the composition of following weight portion: Exocarpium Citri Grandis 300 parts, the processed with honey Radix Stemonae 30 parts, 30 parts of Poria, Rhizoma Pinelliae Preparata 30 parts, Rhizoma Cynanchi Stauntonii 50 parts, 10 parts of Radix Glycyrrhizae, Semen Armeniacae Amarum 100 parts, Fructus Schisandrae Chinensis 20 parts, it is characterized in that, this pharmaceutical composition is prepared from by following methods:
1) Exocarpium Citri Grandis, Semen Armeniacae Amarum vapor distillation, collect distillate, medicinal residues add ethanol extraction, extracting solution crosses neutral alumina, collects effluent, and effluent crosses cationic resin, wash post with water, discard water lotion, use 40%-90% ethanol elution, collecting eluent, resin anion (R.A.) crossed by eluent, washes post with water, discard water lotion, use 40%-90% ethanol elution, collect eluent, concentration, obtains extract A;
2) extracting liquorice, the Rhizoma Pinelliae add ethanol extraction, and extracting solution filters, and filtrate adds the mixing of 3-10% alkali liquor, stands, and filters, discarding precipitation, filtrate adds organic solvent extraction, collects aqueous alkali layer, and pH to 3-4 is adjusted in acid to add 2%, add organic solvent extraction, collect organic solvent layer, reclaim organic solvent, obtain extract B;
3) taking the processed with honey Radix Stemonae, after Poria, Rhizoma Cynanchi Stauntonii, Fructus Schisandrae Chinensis soak, boil extraction, extracting solution filters, and filtrate concentrates, and obtains extract C;
4) united extraction thing A, B, C, dry, to obtain final product.
2. pharmaceutical composition according to claim 1, it is characterized in that, in described step 1), alkali liquor is: in sodium hydroxide, potassium carbonate, potassium bicarbonate, sodium carbonate, sodium bicarbonate, sodium citrate, potassium citrate, sodium sesquicarbonate, sodium dihydrogen citrate any one or several.
3. pharmaceutical composition according to claim 1, it is characterized in that, in described step 1) acid adding adjust pH, wherein acid is: in citric acid, lactic acid, phosphoric acid, tartaric acid, malic acid, metatartaric acid, acetic acid, hydrochloric acid, adipic acid, fumaric acid any one or several.
4. pharmaceutical composition according to claim 1, it is characterized in that, described step 1) cationic resin is: in 732 strongly acidic styrene type cation exchange resins, 734 strongly acidic styrene type cation exchange resins, D254 macroporous strong basic quaternary ammonium cation exchanger resin, D-61 large hole strong acid styrene system cation exchange resin any one or several.
5. pharmaceutical composition according to claim 1, it is characterized in that, in described step 1), resin anion (R.A.) is: in 717 strong-basicity styrene series anion exchange resins, 711 strong-basicity styrene series I type anion exchange resin, D311 macroporous acrylic system weak basic anion exchange resin, D318 macroporous acrylic system weak acid anion exchanger resin one or more.
6. pharmaceutical composition according to claim 1, it is characterised in that described step 2) in organic solvent be: in ethyl acetate, chloroform, normal butane, dichloromethane or ether any one or several.
7. pharmaceutical composition according to claim 1, it is characterised in that this pharmaceutical composition is prepared from by following steps:
1) Exocarpium Citri Grandis, Semen Armeniacae Amarum vapor distillation, collect distillate, medicinal residues add 8-10 times of medical material weight 50%-80% alcohol reflux 1-3 time, each 1-3 hour, united extraction liquid, extracting solution crosses neutral alumina, collect effluent, effluent crosses cationic resin, with the washing post of 2 times of weight resins, discard water lotion, continue with 2 times of weight resin 40%-90% ethanol elutions, collect eluent, eluent continued resin anion (R.A.), with the washing post of 2 times of weight resins, discard water lotion, continue with 2 times of weight resin 40%-90% ethanol elutions, collect eluent, being concentrated into relative density when 60-80 DEG C is 1.1-1.2, obtain extract A;
2) extracting liquorice, Rhizoma Pinelliae 40%-90% alcohol heating reflux extract 1-3 time, the every time ethanol of addition medical material weight 6-10 times, each extraction time is 1-3 hour, filtering, merging filtrate, filtrate adds the sodium carbonate that concentration is 3-10%, stand, filter, discard precipitation, filtrate adds chloroform and extracts 3 times, collects aqueous alkali layer, and the hydrochloric acid that aqueous alkali layer adds 2% adjusts pH to 3-4, chloroform extracts, collect chloroform layer, reclaim chloroform, obtain extract B;
3) take the honey Radix Stemonae, Poria, Rhizoma Cynanchi Stauntonii, Fructus Schisandrae Chinensis added the water soaking of medical material weight 6-10 times after 60 minutes, boiled extraction 1-3 time, and each 1-3 hour, united extraction liquid, filtration, it was 1.1-1.2 that filtrate is concentrated into relative density when 60-80 DEG C, obtains extract C;
4) united extraction thing A, B, C, vacuum drying, to obtain final product.
8. containing the preparation of pharmaceutical composition described in any one of claim 1-6, it is characterised in that said preparation pharmaceutical composition described in any one of claim 1-6 is separately made or is made up of pharmaceutical composition and pharmaceutically acceptable carrier.
CN201610135695.3A 2016-03-10 2016-03-10 Medicine composition with effects of diminishing inflammation and relieving cough and method for preparing medicine composition Pending CN105727104A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107789556A (en) * 2016-08-30 2018-03-13 北京盈科瑞创新医药股份有限公司 A kind of Juhong Tanke Neulized inhalation pharmaceutical solutions and preparation method thereof
WO2023273558A1 (en) * 2021-06-30 2023-01-05 广州白云山星群(药业)股份有限公司 Use of exocarpium citri grandis productive cough extract in preparation of drug for inhibiting human coronavirus infection

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CN1559525A (en) * 2004-02-25 2005-01-05 江苏康缘药业股份有限公司 Red tangerine peel medicine for treating sputum cough and its preparation method
CN1775274A (en) * 2005-02-07 2006-05-24 广东化州中药厂制药有限公司 Cough-relieving sputum-resolving medicinal composition and preparing method
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Publication number Priority date Publication date Assignee Title
CN1559525A (en) * 2004-02-25 2005-01-05 江苏康缘药业股份有限公司 Red tangerine peel medicine for treating sputum cough and its preparation method
CN1775274A (en) * 2005-02-07 2006-05-24 广东化州中药厂制药有限公司 Cough-relieving sputum-resolving medicinal composition and preparing method
CN101181563A (en) * 2006-06-16 2008-05-21 贵州益佰制药股份有限公司 Chrysoidine productive cough preparations as well as preparation method and mass control method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107789556A (en) * 2016-08-30 2018-03-13 北京盈科瑞创新医药股份有限公司 A kind of Juhong Tanke Neulized inhalation pharmaceutical solutions and preparation method thereof
WO2023273558A1 (en) * 2021-06-30 2023-01-05 广州白云山星群(药业)股份有限公司 Use of exocarpium citri grandis productive cough extract in preparation of drug for inhibiting human coronavirus infection

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