CN109045120A - A kind of preparation method and applications of Chinese medical extract that treating nasosinusitis and bronchitis - Google Patents

A kind of preparation method and applications of Chinese medical extract that treating nasosinusitis and bronchitis Download PDF

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CN109045120A
CN109045120A CN201810812353.XA CN201810812353A CN109045120A CN 109045120 A CN109045120 A CN 109045120A CN 201810812353 A CN201810812353 A CN 201810812353A CN 109045120 A CN109045120 A CN 109045120A
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rhizoma
raw material
radix
preparation
root
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严启新
曾琪
季宗念
刘霞
刘程程
金立伟
马安献
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Hai Wang Bai Cao Tang Pharmaceutical Co Ltd
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Hai Wang Bai Cao Tang Pharmaceutical Co Ltd
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/57—Magnoliaceae (Magnolia family)
    • A61K36/575—Magnolia
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
    • A61K36/232—Angelica
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
    • A61K36/236—Ligusticum (licorice-root)
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
    • A61K36/237—Notopterygium
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
    • A61K36/238—Saposhnikovia
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/26—Aristolochiaceae (Birthwort family), e.g. heartleaf
    • A61K36/268—Asarum (wild ginger)
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
    • A61K36/484—Glycyrrhiza (licorice)
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/71—Ranunculaceae (Buttercup family), e.g. larkspur, hepatica, hydrastis, columbine or goldenseal
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P11/00—Drugs for disorders of the respiratory system
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P11/00—Drugs for disorders of the respiratory system
    • A61P11/02—Nasal agents, e.g. decongestants
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation 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
    • A61K2236/30—Extraction of the material
    • A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331—Extraction 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, decoction
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation 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
    • A61K2236/30—Extraction of the material
    • A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation 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
    • A61K2236/30—Extraction of the material
    • A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation 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
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation 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
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation 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
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/55—Liquid-liquid separation; Phase separation

Abstract

The present invention provides the preparation method and applications that " Magnoliae Powder side " (sternly uses and " Yan's prescriptions for succouring sick ", full patent texts abbreviation) Chinese medical extract for the treatment of nasosinusitis and bronchitis from the Song Dynasty.The present invention provides 6 kinds the preparation method comprises the following steps: 1) water extraction method；2) alcohol extracting is followed the example of；3) water extraction and alcohol precipitation method；4) water, which extracts, combines macroporous resin purification method；5) alcohol extracting combination macroporous resin purification method；6) powder mixing method (classics recipe matter basis).6 pairs of party of the invention extract the process optimization of object, are prepared into all kinds of preparations of Chinese medicine, and carry out defining for active part main component.The invention patent provides " Magnoliae Powder side " powder and various traditional Chinese medicine extraction composition oral preparations.And the product of preparation is detected, the Active regenerator clear and definite (by multiple there is certain proportion effective component to form) of Chinese medical extract is embodied, content is higher.

Description

A kind of preparation method and applications of Chinese medical extract that treating nasosinusitis and bronchitis
Technical field
The present invention relates to the preparation method and applications of " Magnoliae Powder side " Chinese medical extract, belong to technical field of Chinese medicine.
Background technique
Rhinitis, that is, nasal cavity inflammatory disease is virus, bacterium, allergen, various physical and chemical factors and certain systemic diseases The inflammation of caused bronchia mucosal.The main pathological change of rhinitis be bronchia mucosal hyperemia, swelling, exudation, hyperplasia, atrophy or Necrosis etc..Its symptom has: nasal obstruction, and nasal obstruction feature is intermittence, and in daytime, day heat, labour or movement, nasal obstruction mitigates, and night Between, nasal obstruction aggravates when sitting quietly or is cold, and another feature of nasal obstruction is alternately.When such as lying on one's side, the congestion of downside is occupied, on Side nasal airflow is good, due to nasal obstruction, or have hyposphresia, headache, giddy, speak in symptoms such as rhinolalia clausas；It is more Tears are often mucus or glutinous purulence, and even at purulence, purulence occurs after being more than secondary infection；Smell decline, mostly two kinds of originals Because caused by, one is schneiderian membrance swelling, nasal obstruction, and air-flow not can enter olfactory region, and two are pierced for regio olfactoria mucous membrane by chronic inflammation for a long time Swash, olfactory function decline or disappearance；Headache, dizzy chronic nasosinusitis show as head heavy feeling more；General manifestation, majority are also There are headache, loss of appetite, easily tired, failure of memory and insomnia etc..Rhinitis is a kind of common disease, and traditional Chinese medicine treats rhinitis Has significant advantage.
The drug of clinical treatment rhinitis has Western medicine and Chinese medicine at present, is oral medicine or aqua nose drops most of in Western medicine, Aqua nose drops easily flow, and are not easy to be attached on nasal membrane, and action time is short, and easy to recur after drug withdrawal, long-time service is easily led to Vasomotor rhinitis；Oral drugs Chinese and Western medicine is added with hormone more, although curative effect is fast, easily repeatedly, long-time service is also easy to produce Drug resistance is big to the side effect of human body.
Magnoliae Powder is sternly used and " reformulating Yan's prescriptions for succouring sick " from the Song Dynasty, " control the deficiency syndrome of the lung, chill dampness and heat in addition, intranasally It is jammed, tears go out endlessly or breath is obstructed or loss of smell." it is right be smalls, it is every to take two money.Tea is taken after mixing with liquid clearly after food.Drug in side Group becomes the flower bud of lily magnolia, asarum (washing away soil, leaf), rhizoma ligustici (going reed), cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae (going to save), windproof (going reed), Rhizoma Et Radix Notopterygii (going reed), Radix Glycyrrhizae (toast), each equal part of the root of Dahurain angelica, cure mainly the deficiency syndrome of the lung, and chill dampness and heat in addition, is intranasally jammed, and tears go out endlessly or gas Obstructed or loss of smell is ceased, is mainly used for the deficiency syndrome of the lung, is attacked outside wind-cold damp pathogen, the illnesss such as be intranasally jammed.The flower bud of lily magnolia, asarum, root of Dahurain angelica hair Dispersing wind and cold, clear the nasal passage are equipped with the chill of Rhizoma Et Radix Notopterygii, radix saposhnikoviae, rhizoma ligustici, cimicifugae foetidae diverging in table, Rhizoma Chuanxiong wind-expelling pain-stopping, caulis akebiae dampness removing Change turbid, Radix Glycyrrhizae coordinating the drug actions of a prescription, shares expelling wind and cold pathogens, the function of clear the nasal passage.
Traditionally, the preparation process of the prescription and instructions of taking are mainly that powder is taken: and traditional powder technological parameter Do not have, it is seen then that traditionally its technique is coarse, and takes, is inconvenient to carry, and dose is big, is also not suitable for being processed into other agent Type.Modern preparation process in relation to Magnoliae Powder, extract research there is no report on document, novel formulation, new drug, and new product is opened Hair and nothing, main active is also blank in research in the embodiment of compound, and flower bud of lily magnolia main component is wood in compound Blue rouge element；Mainly contain Imperatorin in the root of Dahurain angelica；Rhizoma Et Radix Notopterygii mainly contains Notopterol and Isomperatorin, and this patent technique is main to its Ingredient carries out system optimization and confirmation, while having carried out galenic pharmacy research.
Summary of the invention
The purpose of the present invention is overcoming the shortcomings of traditional powder, " Magnoliae Powder side " treatment nasosinusitis and bronchitis are provided The preparation method and applications of Chinese medical extract.
The present invention includes following technical solution:
Technical solution 1: the water for providing " Magnoliae Powder side " Chinese medical extract extracts preparation method, with the flower bud of lily magnolia, asarum, ligusticumic Sheet, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae and the root of Dahurain angelica are raw material, and each raw material relative weight ratio is the flower bud of lily magnolia: asarum: ligusticumic This: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；Preparation method includes as follows Step: above-mentioned ingredients being cleaned, weighs raw material in proportion, and 10~15 times of waters is added to impregnate 20-30min, heating extraction 3 It is secondary, extract 1h for the first time, second extracts 45min, and third time extracts 30min, each extraction time after boiling count It calculates, combined extract, the extracting solution of acquisition is concentrated to 3~5 times that the extracting liquid volume is the raw material weight, obtains just Walk concentrated extracting solution；Being further dried to relative density is 1.0~1.2g/cm3" Magnoliae Powder side " Chinese medical extract.
Technical solution 2: the alcohol extracting preparation method of " Magnoliae Powder side " Chinese medical extract is provided, with the flower bud of lily magnolia, asarum, ligusticumic Sheet, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae and the root of Dahurain angelica are raw material, and each raw material relative weight ratio is the flower bud of lily magnolia: asarum: ligusticumic This: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；Preparation method includes as follows Step: above-mentioned ingredients being cleaned, weighs raw material in proportion, and 10~15 times of 65%~85% ethyl alcohol is added to impregnate 20-30min, Heating and refluxing extraction 2 times, each 1h, combined extract, the volume that extracting solution to the extracting solution of acquisition is concentrated is the original 3~5 times for expecting weight obtain initial concentration extracting solution；Being further dried to relative density is 1.0~1.2g/cm3" the flower bud of lily magnolia Dissipate side " Chinese medical extract.
Technical solution 3: providing the water extract-alcohol precipitation preparation method of " Magnoliae Powder side " Chinese medical extract, with the flower bud of lily magnolia, asarum, Rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae and the root of Dahurain angelica are raw material, and each raw material relative weight ratio is the flower bud of lily magnolia: asarum: Rhizoma ligustici: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；
Preparation method includes the following steps:
1) it prepares concentrate: above-mentioned ingredients being cleaned, weighs raw material in proportion, 10~15 times of waters is added to impregnate 20- 30min heating extraction 3 times, extracts 1h for the first time, and second extracts 45min, and third time extracts 30min, when each extraction Between after boiling calculate, combined extract, it is the raw material weight that the extracting solution of acquisition to the extracting liquid volume, which is concentrated, 3~5 times, obtain initial concentration extracting solution；
2) add ethanol precipitation: adding ethanol in proper amount into the initial concentration extracting solution of above-mentioned preparation, make solvent alcohol content 65 ~75%, 24 hours are stood, filtration, filtrate recycling ethanol obtains refined liquid, is concentrated, is drying to obtain " Magnoliae Powder side " Chinese medicine and mentions Take object.
Technical solution 4: providing the macroporous resin purification preparation method of " Magnoliae Powder side " Chinese medical extract, with the flower bud of lily magnolia, carefully Pungent, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae and the root of Dahurain angelica are raw material, and each raw material relative weight ratio is the flower bud of lily magnolia: thin It is pungent: rhizoma ligustici: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；
Preparation method includes the following steps:
1) it prepares concentrate: above-mentioned ingredients being cleaned, weighs raw material in proportion, 10~15 times of waters is added to impregnate 20- 30min heating extraction 3 times, extracts 1h for the first time, and second extracts 45min, and third time extracts 30min, when each extraction Between after boiling calculate, combined extract, it is the raw material weight that the extracting solution of acquisition to the extracting liquid volume, which is concentrated, 3~5 times, obtain initial concentration extracting solution；
2) it macroporous resin purification: respectively plus in the initial concentration extracting solution that is obtained to upper step of 3~5 times of volume hot water, takes Clear liquid；Supernatant is crossed into macroporous resin column absorption, abandons efflux；Then with the water of 1~5BV with 0.5~2.5BV/ hours stream Speed washs the adsorption column, abandons water lotion；Use 50~70% ethyl alcohol later, 3~5BV of elution volume, with 0.5~ 2.5BV/ hours flow velocitys elute adsorption column, collect the ethanol eluate, and concentration, the dry ethanol eluate obtain " pungent It is smooth to dissipate side " Chinese medical extract.
Technical solution 5: providing the macroporous resin purification preparation method of " Magnoliae Powder side " Chinese medical extract, with the flower bud of lily magnolia, carefully Pungent, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae and the root of Dahurain angelica are made of raw material, and each raw material relative weight ratio is pungent It is smooth: asarum: rhizoma ligustici: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；
Preparation method includes the following steps:
1) it prepares concentrate: taking each taste prepared slices of Chinese crude drugs, weigh raw material in proportion, add 10~15 times of 65%~85% second Alcohol impregnates 20-30min, and heating and refluxing extraction 2 times, each 1h, the extracting solution of acquisition is concentrated to the extraction in combined extract The volume of liquid is 3~5 times of the raw material weight, obtains initial concentration extracting solution；
2) it macroporous resin purification: respectively plus in the initial concentration extracting solution that is obtained to upper step of 3~5 times of volume hot water, takes Clear liquid；Supernatant is crossed into macroporous resin column absorption, abandons efflux；Adsorption column described in the water washing of 5BV is first used after loading, abandons water Washing lotion；Then the adsorption column was washed with 0.5~2.5BV/ hours flow velocitys with the water of 1~5BV, abandons water lotion；It uses later 50~70% ethyl alcohol, 3~5BV of elution volume elute adsorption column with 0.5~2.5BV/ hours flow velocitys, collect the ethyl alcohol and wash De- liquid, concentration, the dry ethanol eluate, obtains " Magnoliae Powder side " Chinese medical extract.
Technical solution 6: providing the preparation method of " Magnoliae Powder side " powder, with the flower bud of lily magnolia, asarum, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, Caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae and the root of Dahurain angelica are made of raw material, and each raw material relative weight ratio is the flower bud of lily magnolia: asarum: rhizoma ligustici: cimicifugae foetidae: river Rhizome of chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；
Preparation method includes the following steps:
Each taste prepared slices of Chinese crude drugs are taken, weigh raw material in proportion, powder is packed to obtain in finely ground mixing sieving.
Technical solution 7: in " Magnoliae Powder side " Chinese medical extract that technical solution of the present invention 1-5 is prepared, contain By weight, magnelin is not less than 0.22%, Imperatorin not less than 0.04%, Notopterol and Isomperatorin total amount for amount Not less than 0.22%, using high performance liquid chromatography (HPLC) measurement by magnelin, Imperatoria ostruthium in the extract that is prepared Element, Notopterol and Isomperatorin total amount content, with not less than for reference substance, measurement is obtained.
Technical solution 8: the oral administration solid of " Magnoliae Powder side " Chinese medical extract being prepared containing the above method is provided Preparation, wherein oral solid formulation includes: tablet, hard capsule, soft capsule, granule, oral solution；Granule, hard capsule and Additive of tablet is selected from starch, Icing Sugar, lactose, dextrin, stevioside, pregelatinized starch, microcrystalline cellulose, calcium bicarbonate, sweet dew The common auxiliary material such as alcohol, hydroxypropyl methyl cellulose, magnesium stearate, superfine silica gel powder, talcum powder, polyethylene glycols；Soft capsule is auxiliary Material is selected from polyethylene glycol (polyethylene glycol 2000-6000), beeswax, atoleine, vegetable oil, glycerol, gelatin etc..Oral solution is auxiliary Material selects beta-cyclodextrin, sorbierite etc., and wherein tablet refers specifically to common compressed tablets, coating tablet, sugar coated tablet, Film coated tablets.
Technical solution 9: it provides " Magnoliae Powder side " Chinese medical extract that the above method is prepared and treats nasosinusitis in preparation And the application in bronchitis drug or health care product.
Illustrate:
In the present invention, the flower bud of lily magnolia used, asarum, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae, root of Dahurain angelica raw material It is their prepared slices of Chinese crude drugs.
In the present invention, the centival % of related ethyl alcohol is concentration expressed in percentage by volume %v/v.
The present invention has following advantages:
1, Chinese medical extract of the invention with the flower bud of lily magnolia, asarum, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae, The root of Dahurain angelica is raw material preparation.Wherein the flower bud of lily magnolia is Magnoliacea plant Magnolia binodii (MagnoliabiondiiPamp.), yulan (MagnoliadenudateDesr.) or sprenger magnolia bark (MagnoliasprengeriPamp.) dry flower, asarum are horse pocket Bell section plant HERBA ASARI from Liaoning of China (AsarumheteroTCMLIBopoidesFr.Schmidtvar.mandshuricum (mAaxim.) Kitag.), asarum (AsarumsieboldiiMiq.) and Seoul asarum (AsarumsieboldiiMiq.f.seoulense (Nakai) C.Y.ChingetC.S.Yang) whole herb with root, rhizoma ligustici be Umbelliferae rhizoma ligustici platymiscium rhizoma ligustici (LigusticumsinenseOliv.) or the dry rhizome of rhizoma ligustici (LigusticumjeholenseNakaietKitag.) And root, cimicifugae foetidae are ranunculaceae plant C.heracleifolia (CimicifugaheracleifoliaKom.), Cimicifuga Dahurica Dry rhizome, the Rhizoma Chuanxiong of (Cimicifugadahurica (Turcz.) Maxim.) or cimicifugae foetidae (CimicifugafoetidaL.) For for umbelliferae Rhizoma Chuanxiong (LigusticumchuanxiongHort.) (or LigusticumwallichiiFranch.) Dry rhizome, caulis akebiae be plants of Lardizabalaceae caulis akebiae (Akebiaquinata (Thunb.) Decne.), threeleaf akebia (Akebiatrifoliata (Thunb.) Koidz.) or caulis akebiae (Akebiatrifoliate (Thunb.) Koidz.var.australis (Diels) Rehd.) drying Teng stem, radix saposhnikoviae be umbelliferae Saposhnikovia divaricata The dry root of (Saposhnikoviadivaricata (Turcz.) Schischk.), Rhizoma Et Radix Notopterygii are umbelliferae Rhizoma Et Radix Notopterygii (back Wing celery) (NotopterygiumincisumTingexH.T.Chang) or notopterygium forbesii (NotopterygiumforbesiiBoiss.) dry rhizome and root, Radix Glycyrrhizae are glycyrrhizic legume (GlycyrrhizauralensisFisch.), swollen fruit Radix (GlycyrrhizainflataBat.) or glycyrrhiza glabra (GlycyrrhizaglabraL.) dry root and rhizome, the root of Dahurain angelica is the umbellate form section plant root of Dahurain angelica (Angelicadahurica (Fisch.exHoffm.) Benth.etHook.f.) or Radix angelicae dahuricae (Angelicadahurica (Fisch.exHoffm.) Benth.etHook.f.var.formosana (Boiss.) ShanetYuan) dry root.The Chinese medical extract of acquisition is institute The mixture that the collaboration containing various active ingredients of medicinal materials works, it is different from activated monomer, and drug effect is living also different from various medicinal materials The simple adduction of property ingredient drug effect.
2, the square Chinese medical extract of " Magnoliae Powder " of the invention is with the flower bud of lily magnolia, asarum, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, anti- Wind, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae, the root of Dahurain angelica are raw material, are sternly used and " Yan Shi through " Magnoliae Powder " prescription known to examination pertinent literature from the Song Dynasty Prescriptions for Succouring the Sick ", specific formula and ratio are as follows, and each raw material relative weight ratio is the flower bud of lily magnolia: asarum: rhizoma ligustici: cimicifugae foetidae: Rhizoma Chuanxiong: wood It is logical: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1.
3, a variety of methods such as present invention employs water to mention, alcohol extracting, water extract-alcohol precipitation, macroporous resin purification, fundamentally guarantee The superiority of " Magnoliae Powder " side traditional Chinese herbal decoction, provides safeguard to be prepared into the different dosage forms product of high quality.It is provided by the invention The preparation process of extract can effectively be enriched with main active such as: before magnelin, Imperatorin, Notopterol and different Europe Plain total amount etc. recklessly.
4, quality control carries out assay using high efficient liquid phase analysis method, simple and easy to control.Extract of the invention Material base is a certain proportion of multiple active component content compositions, still clear to be put forward for the first time active constituent for the formula Material base.Embody the novelty of patent of invention.
5, the various preparation processes extract component obtained and ancient prescription preparation process of extract involved in this patent Compared to (classics recipe matter basis), have effective component high, at low cost, process preparation of being more convenient for convenient for marketing and is answered With.
6, purifying resin method is used in macroporous resin purification preparation method provided by the invention, this method is easy, fast Prompt, favorable reproducibility；Selected macroporous resin adsorption amount is big, and desorption efficiency is big, can Reusability, reduce process costs；Used Etoh solvent is inexpensive nontoxic.The extract that preparation method through macroporous resin purification obtains compared with the decocting object of former prescription, Small in size, Chinese medicine inherent quality height, product moisture absorption is reduced, stability increases, and is easily formed the various dosage forms of appearance looks elegant.
7, the tool of " Magnoliae Powder side " Chinese medical extract prepared by preparation method of the invention treatment nasosinusitis and bronchitis etc. Function.And toxicity is low, has good drug safety, and the clinical of this extract for sufficiently having prompted this technique to prepare is used The safety of medicine.
Therefore, heretofore described " Magnoliae Powder side " square Chinese medical extract is suitble to industrialized production, has very strong reality The property used.
Specific embodiment
Essence of the invention, but do not limit the invention in any way can be better understood by the following examples.
Material source: the flower bud of lily magnolia is Magnoliacea plant Magnolia binodii (MagnoliabiondiiPamp.), asarum is Aristolochiaceae Plant HERBA ASARI from Liaoning of China (AsarumheteroTCMLIBopoidesFr.Schmidtvar.mandshuricum (mAaxim.) Kitag.), asarum (AsarumsieboldiiMiq.) and Seoul asarum (AsarumsieboldiiMiq.f.seoulense (Nakai) C.Y.ChingetC.S.Yang) whole herb with root, rhizoma ligustici be Umbelliferae rhizoma ligustici platymiscium rhizoma ligustici (LigusticumsinenseOliv.) or the dry rhizome of rhizoma ligustici (LigusticumjeholenseNakaietKitag.) And root, cimicifugae foetidae are ranunculaceae plant C.heracleifolia (CimicifugaheracleifoliaKom.), Cimicifuga Dahurica Dry rhizome, the Rhizoma Chuanxiong of (Cimicifugadahurica (Turcz.) Maxim.) or cimicifugae foetidae (CimicifugafoetidaL.) For for umbelliferae Rhizoma Chuanxiong (LigusticumchuanxiongHort.) (or LigusticumwallichiiFranch.) Dry rhizome, caulis akebiae be plants of Lardizabalaceae caulis akebiae (Akebiaquinata (Thunb.) Decne.), threeleaf akebia Teng's stem, the radix saposhnikoviae of (Akebiatrifoliata (Thunb.) Koidz.) or caulis akebiae (AkebiatrifoliateThunb.) For the dry root of umbelliferae Saposhnikovia divaricata (Saposhnikoviadivaricata (Turcz.) Schischk.), Rhizoma Et Radix Notopterygii be for Umbelliferae Rhizoma Et Radix Notopterygii (back wing celery) (NotopterygiumincisumTingexH.T.Chang) or notopterygium forbesii (NotopterygiumforbesiiBoiss.) dry rhizome and root, Radix Glycyrrhizae are glycyrrhizic legume (GlycyrrhizauralensisFisch.), swollen fruit Radix (GlycyrrhizainflataBat.) or glycyrrhiza glabra (GlycyrrhizaglabraL.) dry root and rhizome, the root of Dahurain angelica is the umbellate form section plant root of Dahurain angelica (Angelicadahurica (Fisch.exHoffm.) Benth.etHook.f.) or Radix angelicae dahuricae (Angelicadahurica (Fisch.exHoffm.) Benth.etHook.f.var.formosana (Boiss.) ShanetYuan) dry root.Wherein material passes through business way Diameter purchase.
1 water extracting method of embodiment prepares " Magnoliae Powder side " square Chinese medical extract
Method 1: taking the flower bud of lily magnolia, asarum, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae and the root of Dahurain angelica is raw material, with Water is raw material described in solvent extraction, and each raw material weight ratio is the flower bud of lily magnolia: asarum: rhizoma ligustici: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；Above-mentioned ingredients is cleaned, weighs 50 kilograms of the flower bud of lily magnolia, asarum in proportion 50 kilograms, it is 50 kilograms of rhizoma ligustici, 50 kilograms of cimicifugae foetidae, 50 kilograms of Rhizoma Chuanxiong, 50 kilograms of caulis akebiae, 50 kilograms of radix saposhnikoviae, 50 kilograms of Rhizoma Et Radix Notopterygii, sweet 50 kilograms and 50 kilograms of the root of Dahurain angelica of grass, 5.0 tons of waters impregnate 20min, heating extraction 3 (first time 2h, second of 1h, thirds Secondary 30min, each extraction time after boiling calculate), combined extract, the extracting solution that acquisition is concentrated is mentioned to described Taking liquid product is 3 times of the raw material weight, obtains initial concentration extracting solution；Being further dried to relative density is 1.0g/ cm3" Magnoliae Powder side " Chinese medical extract (lot number 18010106).
Method 2: taking the flower bud of lily magnolia, asarum, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae and the root of Dahurain angelica is raw material, with Water is raw material described in solvent extraction, and each raw material weight ratio is the flower bud of lily magnolia: asarum: rhizoma ligustici: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；Above-mentioned ingredients is cleaned, weighs 65 kilograms of the flower bud of lily magnolia, asarum in proportion 65 kilograms, it is 65 kilograms of rhizoma ligustici, 65 kilograms of cimicifugae foetidae, 65 kilograms of Rhizoma Chuanxiong, 65 kilograms of caulis akebiae, 65 kilograms of radix saposhnikoviae, 65 kilograms of Rhizoma Et Radix Notopterygii, sweet 65 kilograms and 65 kilograms of the root of Dahurain angelica of grass, 6.5 tons of waters impregnate 30min, heating extraction 3 (first time 2h, second of 1h, thirds Secondary 30min, each extraction time after boiling calculate), combined extract, the extracting solution that acquisition is concentrated is mentioned to described Taking liquid product is 5 times of the raw material weight, obtains initial concentration extracting solution；Being further dried to relative density is 1.2g/ cm3" Magnoliae Powder side " Chinese medical extract (lot number 18010208).
Method 3: taking the flower bud of lily magnolia, asarum, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae and the root of Dahurain angelica is raw material, with Water is raw material described in solvent extraction, and each raw material weight ratio is the flower bud of lily magnolia: asarum: rhizoma ligustici: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；Above-mentioned ingredients is cleaned, weighs 75 kilograms of the flower bud of lily magnolia, asarum in proportion 75 kilograms, it is 75 kilograms of rhizoma ligustici, 75 kilograms of cimicifugae foetidae, 75 kilograms of Rhizoma Chuanxiong, 75 kilograms of caulis akebiae, 75 kilograms of radix saposhnikoviae, 75 kilograms of Rhizoma Et Radix Notopterygii, sweet 75 kilograms and 75 kilograms of the root of Dahurain angelica of grass, 7.5 tons of waters impregnate 25min, heating extraction 3 (first time 2h, second of 1h, thirds Secondary 30min, each extraction time after boiling calculate), combined extract, the extracting solution that acquisition is concentrated is mentioned to described Taking liquid product is 4 times of the raw material weight, obtains initial concentration extracting solution；Being further dried to relative density is 1.1g/ cm3" Magnoliae Powder side " Chinese medical extract (lot number 18010309).
2 alcohol extracting method of embodiment prepares " Magnoliae Powder side " Chinese medical extract
Method 1: taking the flower bud of lily magnolia, asarum, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae and the root of Dahurain angelica is raw material, with 65% ethyl alcohol is raw material described in solvent extraction, and each raw material weight ratio is the flower bud of lily magnolia: asarum: rhizoma ligustici: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；Above-mentioned ingredients is cleaned, weigh in proportion 50 kilograms of the flower bud of lily magnolia, 50 kilograms of asarum, 50 kilograms of rhizoma ligustici, 50 kilograms of cimicifugae foetidae, 50 kilograms of Rhizoma Chuanxiong, 50 kilograms of caulis akebiae, 50 kilograms of radix saposhnikoviae, Rhizoma Et Radix Notopterygii 50 are public Jin, 50 kilograms of Radix Glycyrrhizae and 50 kilograms of the root of Dahurain angelica, 5.0 ton of 65% ethyl alcohol impregnate 20min, and heating and refluxing extraction 2 times, each 1h is (every Secondary reflux extracting time after boiling calculate), extracting solution merge, stand 24 hours, supernatant is filtered to take, by supernatant Liquid is concentrated to 3 times of crude drug, obtains initial concentration extracting solution；Being further dried to relative density is 1.0g/cm3" the flower bud of lily magnolia Dissipate side " Chinese medical extract (lot number 18020423).
Method 2: taking the flower bud of lily magnolia, asarum, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae and the root of Dahurain angelica is raw material, with 85% ethyl alcohol is raw material described in solvent extraction, and each raw material weight ratio is the flower bud of lily magnolia: asarum: rhizoma ligustici: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；Above-mentioned ingredients is cleaned, weigh in proportion 65 kilograms of the flower bud of lily magnolia, 65 kilograms of asarum, 65 kilograms of rhizoma ligustici, 65 kilograms of cimicifugae foetidae, 65 kilograms of Rhizoma Chuanxiong, 65 kilograms of caulis akebiae, 65 kilograms of radix saposhnikoviae, Rhizoma Et Radix Notopterygii 65 are public Jin, 65 kilograms of Radix Glycyrrhizae and 65 kilograms of the root of Dahurain angelica, 6.5 ton of 85% ethyl alcohol impregnate 30min, and heating and refluxing extraction 2 times, each 1h is (every Secondary reflux extracting time after boiling calculate), extracting solution merge, stand 24 hours, supernatant is filtered to take, by supernatant Liquid is concentrated to 5 times of crude drug, obtains initial concentration extracting solution；Being further dried to relative density is 1.2g/cm3" the flower bud of lily magnolia Dissipate side " Chinese medicine alcohol extracting thing (lot number 18020524).
Method 3: taking the flower bud of lily magnolia, asarum, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae and the root of Dahurain angelica is raw material, with 75% ethyl alcohol is raw material described in solvent extraction, and each raw material weight ratio is the flower bud of lily magnolia: asarum: rhizoma ligustici: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；Above-mentioned ingredients is cleaned, weigh in proportion 75 kilograms of the flower bud of lily magnolia, 75 kilograms of asarum, 75 kilograms of rhizoma ligustici, 75 kilograms of cimicifugae foetidae, 75 kilograms of Rhizoma Chuanxiong, 75 kilograms of caulis akebiae, 75 kilograms of radix saposhnikoviae, Rhizoma Et Radix Notopterygii 75 are public Jin, 75 kilograms of Radix Glycyrrhizae and 75 kilograms of the root of Dahurain angelica, 7.5 ton of 75% ethyl alcohol impregnate 25min, and heating and refluxing extraction 2 times, each 1h is (every Secondary reflux extracting time after boiling calculate), extracting solution merge, stand 24 hours, supernatant is filtered to take, by supernatant Liquid is concentrated to 4 times of crude drug, obtains initial concentration extracting solution；Being further dried to relative density is 1.1g/cm3" the flower bud of lily magnolia Dissipate side " Chinese medicine alcohol extracting thing (lot number 18020625).
3 water extract-alcohol precipitation method of embodiment prepares " Magnoliae Powder side " Chinese medical extract
Method 1: taking the flower bud of lily magnolia, asarum, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae and the root of Dahurain angelica is raw material, with Water is raw material described in solvent extraction, and each raw material weight ratio is the flower bud of lily magnolia: asarum: rhizoma ligustici: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；Above-mentioned ingredients is cleaned, weighs 50 kilograms of the flower bud of lily magnolia, asarum in proportion 50 kilograms, it is 50 kilograms of rhizoma ligustici, 50 kilograms of cimicifugae foetidae, 50 kilograms of Rhizoma Chuanxiong, 50 kilograms of caulis akebiae, 50 kilograms of radix saposhnikoviae, 50 kilograms of Rhizoma Et Radix Notopterygii, sweet Grass 50 kilograms and 50 kilograms of the root of Dahurain angelica adds 5.0 tons of waters to impregnate 20min, heating extraction 3 times (first time 2h, second of 1h, the 30min three times, each extraction time after boiling calculate), the extracting solution of acquisition is concentrated to described in combined extract Extracting liquid volume is 3 times of the raw material weight, obtains initial concentration extracting solution；It is slowly added to ethanol in proper amount while stirring, makes Solvent alcohol content is 65%, stands 24 hours, and filtration, filtrate recycling ethanol obtains refined liquid, is concentrated, dry to obtain the " flower bud of lily magnolia Dissipate side " Chinese medical extract (lot number 18030518).
Method 2: taking the flower bud of lily magnolia, asarum, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae and the root of Dahurain angelica is raw material, with Water is raw material described in solvent extraction, and each raw material weight ratio is the flower bud of lily magnolia: asarum: rhizoma ligustici: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；Above-mentioned ingredients is cleaned, weighs 65 kilograms of the flower bud of lily magnolia, asarum in proportion 65 kilograms, it is 65 kilograms of rhizoma ligustici, 65 kilograms of cimicifugae foetidae, 65 kilograms of Rhizoma Chuanxiong, 65 kilograms of caulis akebiae, 65 kilograms of radix saposhnikoviae, 65 kilograms of Rhizoma Et Radix Notopterygii, sweet Grass 65 kilograms and 65 kilograms of the root of Dahurain angelica adds 6.5 tons of waters to impregnate 30min, heating extraction 3 times (first time 2h, second of 1h, the 30min three times, each extraction time after boiling calculate), the extracting solution of acquisition is concentrated to described in combined extract Extracting liquid volume is 5 times of the raw material weight, obtains initial concentration extracting solution；It is slowly added to ethanol in proper amount while stirring, makes Solvent alcohol content is 75%, stands 24 hours, and filtration, filtrate recycling ethanol obtains refined liquid, is concentrated, dry to obtain the " flower bud of lily magnolia Dissipate side " Chinese medical extract (lot number 18030620).
Method 3: taking the flower bud of lily magnolia, asarum, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae and the root of Dahurain angelica is raw material, with Water is raw material described in solvent extraction, and each raw material weight ratio is the flower bud of lily magnolia: asarum: rhizoma ligustici: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；Above-mentioned ingredients is cleaned, weighs 75 kilograms of the flower bud of lily magnolia, asarum in proportion 75 kilograms, it is 75 kilograms of rhizoma ligustici, 75 kilograms of cimicifugae foetidae, 75 kilograms of Rhizoma Chuanxiong, 75 kilograms of caulis akebiae, 75 kilograms of radix saposhnikoviae, 75 kilograms of Rhizoma Et Radix Notopterygii, sweet Grass 75 kilograms and 75 kilograms of the root of Dahurain angelica adds 7.5 tons of waters to impregnate 25min, heating extraction 3 times (first time 2h, second of 1h, the 30min three times, each extraction time after boiling calculate), the extracting solution of acquisition is concentrated to described in combined extract Extracting liquid volume is 4 times of the raw material weight, obtains initial concentration extracting solution；It is slowly added to ethanol in proper amount while stirring, makes Solvent alcohol content is 70%, stands 24 hours, and filtration, filtrate recycling ethanol obtains refined liquid, is concentrated, dry to obtain the " flower bud of lily magnolia Dissipate side " Chinese medical extract (lot number 18030722).
4 macroporous resin method one of embodiment prepares " Magnoliae Powder side " Chinese medical extract
Method 1: taking the flower bud of lily magnolia, asarum, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae and the root of Dahurain angelica is raw material, with Water is raw material described in solvent extraction, and each raw material weight ratio is the flower bud of lily magnolia: asarum: rhizoma ligustici: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；Above-mentioned ingredients is cleaned, weighs 50 kilograms of the flower bud of lily magnolia, asarum in proportion 50 kilograms, it is 50 kilograms of rhizoma ligustici, 50 kilograms of cimicifugae foetidae, 50 kilograms of Rhizoma Chuanxiong, 50 kilograms of caulis akebiae, 50 kilograms of radix saposhnikoviae, 50 kilograms of Rhizoma Et Radix Notopterygii, sweet 50 kilograms and 50 kilograms of the root of Dahurain angelica of grass, 5.0 tons of waters impregnate 20min, heating extraction 3 (first time 2h, second of 1h, thirds Secondary 30min, each extraction time after boiling calculate), combined extract, the extracting solution that acquisition is concentrated is mentioned to described Taking liquid product is 3 times of the raw material weight, obtains initial concentration extracting solution；Add 3 times of hot water dilute initial concentration extracting solution It releases, appropriate Chinese medicine clarifying agent chitosan is added, be centrifuged, go to precipitate, take supernatant, be splined on D101 macroporous resin column (in loading It is preceding respectively with acid, alkali, water, alcohol carries out pre-treatment to resin column), 1BV pure water rinsing is first used after loading, aqueous solution reject is used instead 50% ethanol elution of 3BV, eluent flow rate 0.5BV/h collect the ethanol eluate.Continue that solvent is recovered under reduced pressure, collects Medicinal extract, it is dry to obtain " Magnoliae Powder side " Chinese medical extract (lot number 18040817).
Method 2: taking the flower bud of lily magnolia, asarum, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae, the root of Dahurain angelica is raw material, with water For raw material described in solvent extraction, each raw material weight ratio is the flower bud of lily magnolia: asarum: rhizoma ligustici: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: sweet Grass: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；Above-mentioned ingredients is cleaned, weighs 65 kilograms of the flower bud of lily magnolia, asarum 65 in proportion Kilogram, 65 kilograms of rhizoma ligustici, 65 kilograms of cimicifugae foetidae, 65 kilograms of Rhizoma Chuanxiong, 65 kilograms of caulis akebiae, windproof 65 kilograms, 65 kilograms of Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae 65 kilograms, 65 kilograms of the root of Dahurain angelica, 6.5 tons of waters impregnate 30min, heating extraction 3 (first time 2h, second of 1h, third times 30min, each extraction time after boiling calculate), the extracting solution of acquisition is concentrated to the extraction in combined extract Liquid product is 5 times of the raw material weight, obtains initial concentration extracting solution；Initial concentration extracting solution is added into 5 times of hot water dilutions, Appropriate Chinese medicine clarifying agent chitosan is added, is centrifuged, goes to precipitate, take supernatant, be splined on D101 macroporous resin column (before loading Respectively with acid, alkali, water, alcohol carries out pre-treatment to resin column), 5BV pure water rinsing is first used after loading, aqueous solution reject is used instead 70% ethanol elution of 5BV, eluent flow rate 2.5BV/h collect the ethanol eluate.Continue that solvent is recovered under reduced pressure, collects Medicinal extract, it is dry to obtain " Magnoliae Powder side " Chinese medical extract (lot number 18040927).
Method 3: taking the flower bud of lily magnolia, asarum, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae, the root of Dahurain angelica is raw material, with water For raw material described in solvent extraction, each raw material weight ratio is the flower bud of lily magnolia: asarum: rhizoma ligustici: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: sweet Grass: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；Above-mentioned ingredients is cleaned, weighs 75 kilograms of the flower bud of lily magnolia, asarum 75 in proportion Kilogram, 75 kilograms of rhizoma ligustici, 75 kilograms of cimicifugae foetidae, 75 kilograms of Rhizoma Chuanxiong, 75 kilograms of caulis akebiae, windproof 75 kilograms, 75 kilograms of Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae 75 kilograms, 75 kilograms of the root of Dahurain angelica, 7.5 tons of waters impregnate 25min, heating extraction 3 (first time 2h, second of 1h, third times 30min, each extraction time after boiling calculate), the extracting solution of acquisition is concentrated to the extraction in combined extract Liquid product is 4 times of the raw material weight, obtains initial concentration extracting solution；Initial concentration extracting solution is added into 4 times of hot water dilutions, Appropriate Chinese medicine clarifying agent chitosan is added, is centrifuged, goes to precipitate, take supernatant, be splined on D101 macroporous resin column (before loading Respectively with acid, alkali, water, alcohol carries out pre-treatment to resin column), 2.5BV pure water rinsing is first used after loading, aqueous solution reject is used instead 60% ethanol elution of 4BV, eluent flow rate 1.5BV/h collect the ethanol eluate.Continue that solvent is recovered under reduced pressure, collects Medicinal extract, it is dry to obtain " Magnoliae Powder side " Chinese medical extract (lot number 18041021).
5 macroporous resin method two of embodiment prepares " Magnoliae Powder side " Chinese medical extract
Method 1: taking the flower bud of lily magnolia, asarum, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae, the root of Dahurain angelica is raw material, with 65% ethyl alcohol is raw material described in solvent extraction, and each raw material weight ratio is the flower bud of lily magnolia: asarum: rhizoma ligustici: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；Above-mentioned ingredients is cleaned, weigh in proportion 50 kilograms of the flower bud of lily magnolia, 50 kilograms of asarum, 50 kilograms of rhizoma ligustici, 50 kilograms of cimicifugae foetidae, 50 kilograms of Rhizoma Chuanxiong, 50 kilograms of caulis akebiae, 50 kilograms of radix saposhnikoviae, Rhizoma Et Radix Notopterygii 50 are public Jin, 50 kilograms of Radix Glycyrrhizae, 50 kilograms of the root of Dahurain angelica, 5.0 ton of 65% ethyl alcohol impregnate 20min, and heating and refluxing extraction 2 times, each 1h is (every time Reflux extracting time after boiling calculate), extracting solution merge, stand 24 hours, supernatant is filtered to take, by supernatant 3 times of crude drug are concentrated to, initial concentration extracting solution is obtained；By concentrated extracting solution plus 3 times of hot water dilutions, appropriate Chinese medicine is added Clarifying agent chitosan, centrifugation, go to precipitate, take supernatant, be splined on D101 macroporous resin column (before loading respectively with acid, alkali, Water, alcohol carry out pre-treatment to resin column), the adsorption column first is washed with 5BV water (being 5 with 1% hydrochloric acid adjusting PH) after loading, Abandon water lotion；It is eluted again with neutrality 1BV aqueous solution, aqueous solution reject uses 50% ethanol elution of 3BV instead, and elution flow rate is 0.5BV/h collects the ethanol eluate.Continue that solvent is recovered under reduced pressure, collect medicinal extract, dry " Magnoliae Powder side " Chinese medicine that obtains mentions Take object (lot number 18051103).
Method 2: taking the flower bud of lily magnolia, asarum, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae, the root of Dahurain angelica is raw material, with 85% ethyl alcohol is raw material described in solvent extraction, and each raw material weight ratio is the flower bud of lily magnolia: asarum: rhizoma ligustici: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；Above-mentioned ingredients is cleaned, weigh in proportion 65 kilograms of the flower bud of lily magnolia, 65 kilograms of asarum, 65 kilograms of rhizoma ligustici, 65 kilograms of cimicifugae foetidae, 65 kilograms of Rhizoma Chuanxiong, 65 kilograms of caulis akebiae, 65 kilograms of radix saposhnikoviae, Rhizoma Et Radix Notopterygii 65 are public Jin, 65 kilograms of Radix Glycyrrhizae, 65 kilograms of the root of Dahurain angelica, 6.5 ton of 85% ethyl alcohol impregnate 30min, and heating and refluxing extraction 2 times, each 1h is (every time Reflux extracting time after boiling calculate), extracting solution merge, stand 24 hours, supernatant is filtered to take, by supernatant 5 times of crude drug are concentrated to, initial concentration extracting solution is obtained；By concentrated extracting solution plus 5 times of hot water dilutions, appropriate Chinese medicine is added Clarifying agent chitosan, centrifugation, go to precipitate, take supernatant, be splined on D101 macroporous resin column (before loading respectively with acid, alkali, Water, alcohol carry out pre-treatment to resin column), the adsorption column first is washed with 5BV water (being 6 with 1% hydrochloric acid adjusting PH) after loading, Abandon water lotion；It is eluted again with neutrality 5BV aqueous solution, aqueous solution reject uses 70% ethanol elution for washing 5BV, elution flow rate instead For 2.5BV/h, the ethanol eluate is collected.Continue that solvent is recovered under reduced pressure, collects medicinal extract, it is dry to obtain " Magnoliae Powder side " Chinese medicine Extract (lot number 18051205).
Method 3: taking the flower bud of lily magnolia, asarum, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae, the root of Dahurain angelica is raw material, with 75% ethyl alcohol is raw material described in solvent extraction, and each raw material weight ratio is the flower bud of lily magnolia: asarum: rhizoma ligustici: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；Above-mentioned ingredients is cleaned, weigh in proportion 75 kilograms of the flower bud of lily magnolia, 75 kilograms of asarum, 75 kilograms of rhizoma ligustici, 75 kilograms of cimicifugae foetidae, 75 kilograms of Rhizoma Chuanxiong, 75 kilograms of caulis akebiae, 75 kilograms of radix saposhnikoviae, Rhizoma Et Radix Notopterygii 75 are public Jin, 75 kilograms of Radix Glycyrrhizae, 75 kilograms of the root of Dahurain angelica, 7.5 ton of 75% ethyl alcohol impregnate 25min, and heating and refluxing extraction 2 times, each 1h is (every time Reflux extracting time after boiling calculate), extracting solution merge, stand 24 hours, supernatant is filtered to take, by supernatant 4 times of crude drug are concentrated to, initial concentration extracting solution is obtained；By concentrated extracting solution plus 4 times of hot water dilutions, appropriate Chinese medicine is added Clarifying agent chitosan, centrifugation, go to precipitate, take supernatant, be splined on D101 macroporous resin column (before loading respectively with acid, alkali, Water, alcohol carry out pre-treatment to resin column), the absorption first is washed with 5BV water (being 5.5 with 1% hydrochloric acid adjusting PH) after loading Column abandons water lotion；It is eluted again with neutrality 3BV aqueous solution, aqueous solution reject, uses 60% ethanol elution for washing 4BV, elution stream instead Speed is 1.5BV/h, collects the ethanol eluate.Continue that solvent is recovered under reduced pressure, collects medicinal extract, it is dry to obtain in " Magnoliae Powder side " Medicament extract (lot number 18051228).
Embodiment 6 " Magnoliae Powder side " powder
Method: taking the flower bud of lily magnolia, asarum, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae and the root of Dahurain angelica is raw material, each original Material weight ratio is 1:1:1:1:1:1:1:1:1:1；Above-mentioned ingredients is cleaned into finely ground mixing sieving packaging into (lot number is 18061118)。
The oral preparation preparation method of embodiment 7 " Magnoliae Powder side " Chinese medical extract
1) preparation of " Magnoliae Powder side " Chinese medical extract granule
Prescription: (Magnoliae Powder extract is taken respectively from embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5 " Magnoliae Powder " square Chinese medical extract)
Magnoliae Powder extract: 500.0g
Starch: 200.0g
Calcium monohydrogen phosphate: 150.0g
Dextrin: 100.0g
Lactose: 50.0g
Recipe quantity Magnoliae Powder extract is weighed, the auxiliary material of recipe quantity is added, adds 60% ethyl alcohol softwood, crosses the granulation of 20 mesh, 50~60 DEG C of forced air dryings (moisture control is 5%~8%) cross 16 mesh sieves to get flower bud of lily magnolia scattered seed.
2) preparation of " Magnoliae Powder side " Chinese medical extract coating tablet
Prescription: (Magnoliae Powder extract is taken respectively from embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5 " Magnoliae Powder " square Chinese medical extract)
Magnoliae Powder extract: 500.0g
Pregelatinized starch: 200.0g
Microcrystalline cellulose: 230.0g
Stevioside: 25.0g
Sucrose: 25.0g
Magnesium stearate: 10.0g
Superfine silica gel powder: 10.0g
Coating agent: promise coloured silk TM coating agent soluble in the stomach (appropriate)
The Magnoliae Powder extract for weighing recipe quantity is added the auxiliary material (magnesium stearate, superfine silica gel powder are additional) of recipe quantity, adds 60% ethyl alcohol softwood crosses the granulation of 20 mesh, and 50~60 DEG C of forced air dryings (moisture control is 5%~8%) cross 16 mesh sieves, It is uniformly mixed, tabletting, is coated to get Magnoliae Powder coating tablet with additional auxiliary material magnesium stearate, superfine silica gel powder.
3) preparation of " Magnoliae Powder side " Chinese medical extract capsule
Prescription: (Magnoliae Powder extract is taken respectively from embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5 " Magnoliae Powder " square Chinese medical extract)
Magnoliae Powder extract: 500.0g
Hydroxypropyl methylcellulose: 40.0g (adds) in the additional half of half
Pregelatinized starch: 190.0g
Microcrystalline cellulose: 200.0g
Lactose: 25.0g
Icing Sugar: 25.0g
Magnesium stearate: 10.0g
Talcum powder: 10.0g
Recipe quantity Magnoliae Powder extract is weighed, the auxiliary material (magnesium stearate, talcum powder are additional) of recipe quantity is added, adds 60% Ethyl alcohol softwood crosses the granulation of 20 mesh, and 50~60 DEG C of forced air dryings (moisture control is 5%~8%) cross 16 mesh sieves, and outer Add auxiliary material magnesium stearate, superfine silica gel powder to be uniformly mixed, is filled with filling machine to get flower bud of lily magnolia powder capsule.
4) preparation of " Magnoliae Powder side " Chinese medical extract soft capsule
Prescription: (Magnoliae Powder extract is taken respectively from embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5 " Magnoliae Powder " square Chinese medical extract)
Magnoliae Powder extract: 500.0g
Vegetable oil: 140.0g
Sorbierite: 100.0g
Glycerol: 50.0g
Atoleine: 60.0g
Gelatin: 150.0g
It weighs recipe quantity Magnoliae Powder extract to be uniformly mixed with the vegetable oil of recipe quantity, sorbierite, by gelatin and glycerol point It is not contained in hopper, two liquid are sprayed by the double-deck spray head of concentric tube-shaped with friction speed, make a certain amount of glue by one It after quantitative medical fluid package, instills in another coolant liquid (atoleine) that do not dissolve each other mutually, because of table after glue contact coolant liquid Face tension force effect becomes spherical, and gradually solidification forms soft capsule.
5) preparation of " Magnoliae Powder side " Chinese medical extract oral solution
Prescription: (Magnoliae Powder extract is taken respectively from embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5 " Magnoliae Powder " square Chinese medical extract)
Magnoliae Powder extract: 500.0g
Beta-cyclodextrin: 140.0g
Sucrose: 100.0g
Distilled water 260.0g
Recipe quantity Magnoliae Powder extract is weighed, the auxiliary material of recipe quantity is added, distilled water is added to dissolve, stirs evenly to get pungent Smooth scattered extract oral liquid.
The determination of bioactive constituent of embodiment 8 " Magnoliae Powder side " extract and powder
1. chromatographic condition
Agilent1260 high performance liquid chromatograph, UV detector (DAD) are to fill out with octadecylsilane chemically bonded silica Fill agent, C18 chromatographic column (4.6mm × 250mm, 5 μm)；Magnelin (National Institute for Food and Drugs Control, lot number: Detection wavelength 110773-20101): 278nm, mobile phase: acetonitrile-tetrahydrofuran-water (35:1:64)；Imperatorin (China Food and medicine examine and determine research institute, lot number: 110663-20201) Detection wavelength: 300nm, mobile phase: methanol-water (55:45)； Notopterol (National Institute for Food and Drugs Control, lot number: 110763-20201) and Isomperatorin (Chinese drug biology system Institute is determined in product examine, lot number: 110709-201206) Detection wavelength of total amount: 310nm, mobile phase: acetonitrile-water (44:56)；Flow velocity: 1.0ml/min；Column temperature: 30 DEG C；Sample volume: 10 μ l.
The preparation of " 2. Magnoliae Powder side " Chinese medical extract sample
1) extract of the present invention
Each 1 lot number of above-mentioned Chinese medical extract is made respectively by method described in present example 1,2,3,4,5,6.
3. the preparation of standard solution
Take magnelin reference substance appropriate, it is accurately weighed, add methanol be made solution of every lml containing 0.1mg to get；Take Europe Peucedanin reference substance is appropriate, accurately weighed, add methanol be made every lmL containing 10 μ g solution to get；Take Notopterol, different Imperatoria ostruthium Plain reference substance is appropriate, accurately weighed, add methanol be made every lmL contain respectively 60 μ g, 30 μ g solution to get.
4. measuring method
Take the above-mentioned Chinese medical extract sample of each lot number appropriate respectively, accurately weighed about 10-25mg is transferred to 50ml appearance In measuring bottle, add methanol 40ml, ultrasound 30min under room temperature, taking-up is cooled to room temperature, and methanol is added to shake up to scale, draw it is appropriate, It is settled to 50ml, is shaken up, can be measured.Each component content is calculated according to one point external standard method.It the results are shown in Table 1:
1 Magnoliae Powder extract of table and powder each component assay result
Therefore " Magnoliae Powder side " Chinese medical extract and its powder, contain by weight, magnelin not less than 0.22%, Imperatorin is not less than 0.22% not less than 0.04%, Notopterol and Isomperatorin total amount.
The anti-inflammatory experimental study of embodiment 8 " Magnoliae Powder side " Chinese medical extract
Note kunming mice 180, sub-model group, anti-inflammatory be logical, sample 1-1 (lot number: 18010106), sample 1-2 (lot number: 18010208), sample 1-3 (lot number: 18010309), sample 2-1 (lot number: 18020423), sample 2-2 (lot number: 18020524), sample 2-3 (lot number: 18020625), sample 3-1 (lot number: 18030518), sample 3-2 (lot number: 18030620), sample 3-3 (lot number: 18030722), sample 4-1 (lot number: 18040817), sample 4-2 (lot number: 18040927), sample 4-3 (lot number: 18041021), sample 5-1 (lot number: 18051103), sample 5-2 (lot number: 18051205), sample 5-3 (lot number: 18051228), sample 6-1, (lot number: 18061118) totally ten eight groups.Every group of animal is each 10, each group mouse continuous gavage is administered 10 days, only causes inflammation in mouse right ear coating dimethylbenzene 0.02ml/ after the last administration.Between Cervical dislocation puts to death mouse after 3h, cuts ears along auricle base line, is beaten with diameter 8mm punch at the same position of two ears Lower auricle is simultaneously weighed.It the results are shown in Table 2.
Compared with model group, positive controls, sample 1-1,1-2,1-3,2-1,2-2,2-3,3-1,3-2,3-3,4-1, 4-2,4-3,5-1,5-2,5-3,6-1 have extremely significant difference (p < 0.05) to mouse ear swelling degree and negative control group；Illustrate each The significant anti-inflammatory effect of sample, meanwhile, sample 4-1,4-2,4-3,5-1,5-2,5-3,6-1 antiphlogistic effects are better than sample 1- 1,1-2,1-3,2-1,2-2,2-3,3-1,3-2,3-3.
The influence of 2 paraxylene of table cause mouse ear swelling
Group Dosage (g/kg) Swelling (mg)
Model group —— 7.05±2.12
Anti-inflammatory is logical 2.000 3.25±1.45***
Sample 1-1 1.400 6.49±1.12*
Sample 1-2 1.400 6.46±1.26*
Sample 1-3 1.400 6.42±1.33*
Sample 2-1 1.100 6.62±1.12*
Sample 2-2 1.100 6.58±1.06*
Sample 2-2 1.100 6.66±1.21*
Sample 3-1 0.900 5.01±1.17*
Sample 3-2 0.900 5.08±1.04*
Sample 3-3 0.900 5.09±1.34*
Sample 4-1 0.530 4.39±1.23**
Sample 4-2 0.530 4.32±1.19**
Sample 4-3 0.530 4.35±1.08**
Sample 5-1 0.450 4.12±1.37**
Sample 5-2 0.450 4.17±1.46**
Sample 5-3 0.450 4.18±1.18**
Sample 6-1 0.460 4.20±1.04**
Compared with model group, p < 0.05 *；**p<0.01；***p<0.001
The treatment bronchitis experimental study of embodiment 9 " Magnoliae Powder side " Chinese medical extract
1 material and instrument
1.1 experimental animal
7 kind healthy mice 200, week old female cleaning grade Kunming, weight (20 ± 2) g, by The Fourth Military Medical University's reality Animal center offer, credit number: SCXK (army) word the 2012-005th are provided.
1.2 drug
Embodiment 1-6 prepares sample, sample 1-1 (lot number: 18010106), sample 1-2 (lot number: 18010208), sample 1-3 (lot number: 18010309), sample 2-1 (lot number: 18020423), sample 2-2 (lot number: 18020524), sample 2-3 (batch Number: 18020625), sample 3-1 (lot number: 18030518), sample 3-2 (lot number: 18030620), sample 3-3 (lot number: 18030722), sample 4-1 (lot number: 18040817), sample 4-2 (lot number: 18040927), sample 4-3 (lot number: 18041021), sample 5-1 (lot number: 18051103), sample 5-2 (lot number: 18051205), sample 5-3 (lot number: 18051228), sample 6-1 (lot number: 18061118)
1.3 reagent
Superoxide dismutase (SOD) kit, lot number: 20161209, total antioxidant capacity (T-AOC) kit, batch Number: 20161209, Coomassie brilliant blue kit, lot number: 20161219, Bioengineering Research Institute is built up purchased from Nanjing；Tumour is bad Necrosis factor (TNF-α) detection kit, lot number: 1511061, interleukin 10 (IL-10) detection kit, lot number: 1511292, P&D company of the U.S. develops (import packing)；Ethyl alcohol, lot number: 1506073301, Anhui An Te biological products are limited Company；Petroleum ether, lot number: 20151222, Tianjin chemical reagent Co., Ltd；Chloroform, lot number: 20170115, traditional Chinese medicines collection Chemical reagent Co., Ltd of group；Ethyl acetate, lot number: 20150228, Tianjin chemical reagent Co., Ltd；N-butanol, lot number: 20160430, Tianjin Jinbei Fine Chemicals Co., Ltd..The above reagent is that analysis is pure.
1.4 key instrument
MODEL680 type microplate reader；722 type ultraviolet light spectrophotometers；RE5205 type rotary evaporator；Refrigerated centrifuge Machine；Eddy blending machine；20~1000 μ L micropipettors, homogenizer, electronic balance, surgical instrument etc..
2 methods
2.1 animal packet
200 female mices are randomly divided into: Normal group, model group, GUILONG KECHUANNING JIAONANG positive controls, Self-healing group, embodiment 1-6 prepare 16 groups of sample, and totally 20 groups, every group 20.
2 modeling methods
Ammonium hydroxide stimulation causes murine chronic bronchitis model.It is multi-functional that mouse is successively put into YIS-8A as unit of group Instrument to induce to cough and asthma draws cough method inducing mouse using ammonia atomization sucking and generates chronic bronchitis.In addition to Normal group, Remaining each group every bu morning and afternoon gives ammonia atomization and sucks 5 times, each 2min, is spaced 30min, total 30d.
2.3 administration
In addition to normal group and self-healing group, drug treatment after remaining 18 groups of mouse ammonium hydroxide stimulation 30d, sample sets grouping according to Dosage 4g/kg administration；GUILONG KECHUANNING JIAONANG suspension group is administered by 1g/kg；Each group intragastric administration on mice equal 1 time/d, continuous 15d.
2.4 Indexs measure
Pluck eyeball after morning dose 2h and take blood within each group mouse after administration the 15th day, be placed in refrigerated centrifuge with 4 DEG C, 4000r/min is centrifuged 10min and separates serum, and -20 DEG C of preservations are to be checked.It weighs simultaneously and organizes about 0.2g in the middle part of every mouse right lung, 10% lung homogenate is made of 4 DEG C of physiological saline, 4 DEG C, 4000r/min centrifugation 10min extract supernatant and freeze in -20 DEG C It saves to be checked.While prepared by serum and lung tissue sample, left side central portion is taken, lung tissue block about 4mm × 4mm size is used The infiltration of 10% formalin, fixed, conventional to be dehydrated, paraffin embedding, slice, with a thickness of 4 μm, row HE dyeing prepares pathology and cuts Piece.Items detection is carried out in strict accordance with kit specification.
2.5 statistical procedures
Detection gained continuous data is indicated with x ± s, is handled using SPSS15.0 statistical analysis software.Comparison among groups It is examined using variance analysis and LSD-t.
3 results
Influence of 3.1 sample sets to mouse lung tissue SOD, T-AOC and Serum TNF-α, IL-10
Compared with Normal group, model group mouse lung tissue T-AOC, SOD activity significantly reduces (P < 0.01), TNF- The horizontal significant raising (P < 0.01) of α, IL-10；Compared with model group, sample sets mouse lung tissue T-AOC activity is significant to increase (P < 0.01), SOD activity is significant increases (P < 0.05 or P < 0.01), and Serum TNF-α, IL-10 level significantly reduce (P < 0.05 or P <0.01).It is shown in Table 2.
3 sample sets of table to mouse lung tissue SOD, T-AOC and Serum TNF-α, IL-10 influence (
N=10)
Note: compared with normal group,*P < 0.05,*P<0.01；Compared with model group,#P < 0.05,##P<0.01
Conclusion: illustrating that each sample significantly treats bronchitis effect, meanwhile, sample 4-1,4-2,4-3,5-1,5-2, 5-3 treatment bronchitis effect is better than sample 1-1,1-2,1-3,2-1,2-2,2-3,3-1,3-2,3-3, sample 6-1 treatment Bronchitis effect is worst.
The acute toxicological experiment of embodiment 10 " Magnoliae Powder side " extract
Preliminary experiment: pressing acute toxicological experiment method, selects kunming mice 20, water 12h is can't help in fasting.Embodiment 1 (lot number: extract is configured to the suspension of maximum concentration in 18010106).The each stomach-filling of every mouse is about 0.8mL/20g (weight) interior stomach-filling 3 times for 24 hours, is spaced 4h.Then it routinely raises, and observes toxic reaction situation (appearance, work of mouse Dynamic, breathing, secretion, defecation, death etc.), and continuous weighting 7 days.Because capacity is administered with maximum administration concentration, maximum, not Median lethal dose (LD50) is measured, therefore does maximum dosage-feeding experiment.
1) general performance
After administration in 14 days, the equal diet of experimental mice is normal, and fur is smooth, and freely, stool and urine is normal, is no different for activity Normal secretion, respiratory system, cardiovascular system, nervous system, digestive system and urinary system are showed no exception, and mouse is complete Portion's survival.Its daily maximum dosage-feeding is that per kilogram is 250g.
2) changes of weight situation
After administration in 14 days, weight variation without exception.
3) main organs are observed
2 groups of mouse are through gross anatomy and observe by the naked eye, and have no the abnormal phenomenon such as internal organs enlargement, atrophy, necrosis, main Want internal organs without any bad lesion, it is close with blank control group, illustrate embodiment 1 (lot number: in 18010106) extract without Poison, synchronization can reasoning illustrate that other each sample groups are also nontoxic (other each sample group prescriptions are consistent, are only process reforms).It is comprehensive It is upper described, prompt this medicine nontoxic, clinical dosage is the dosage of a safety, clinical application safety.

Claims (9)

1. the water of " Magnoliae Powder side " Chinese medical extract extracts preparation method, which is characterized in that with the flower bud of lily magnolia, asarum, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae and the root of Dahurain angelica are made of each equal part of raw material；Each raw material relative weight ratio is the flower bud of lily magnolia: asarum: ligusticumic This: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；
Preparation method includes the following steps: to take each taste prepared slices of Chinese crude drugs, weighs raw material in proportion, 10~15 times of waters is added to impregnate 20-30min heating extraction 3 times, extracts 1h, second of extraction 45min for the first time, and third time extracts 30min, each extraction Time after boiling calculate, combined extract, it is the raw material weight that the extracting solution of acquisition to the extracting liquid volume, which is concentrated, 3~5 times of amount obtain initial concentration extracting solution；Being further dried to relative density is 1.0~1.2g/cm3" Magnoliae Powder side " Chinese medical extract.
The alcohol extracting preparation method of " 2. Magnoliae Powder side " Chinese medical extract, which is characterized in that with the flower bud of lily magnolia, asarum, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae and the root of Dahurain angelica are made of each equal part of raw material；Each raw material relative weight ratio is the flower bud of lily magnolia: asarum: ligusticumic This: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；
Preparation method includes the following steps: to take each taste prepared slices of Chinese crude drugs, weighs raw material in proportion, add 10~15 times 65%~85% Ethyl alcohol impregnates 20-30min, and heating and refluxing extraction 2 times, each 1h, the extracting solution of acquisition is concentrated to the extraction in combined extract The volume of liquid is 3~5 times of the raw material weight, obtains initial concentration extracting solution；Be further dried to relative density be 1.0~ 1.2g/cm3" Magnoliae Powder side " Chinese medical extract.
The water extract-alcohol precipitation preparation method of " 3. Magnoliae Powder side " Chinese medical extract, which is characterized in that with the flower bud of lily magnolia, asarum, rhizoma ligustici, liter Fiber crops, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae and the root of Dahurain angelica are made of each equal part of raw material；Each raw material relative weight ratio is the flower bud of lily magnolia: thin It is pungent: rhizoma ligustici: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；
Preparation method includes the following steps:
1) it prepares concentrate: above-mentioned ingredients being cleaned, weighs raw material in proportion, 10~15 times of waters is added to impregnate 20- 30min heating extraction 3 times, extracts 1h, second of extraction 45min for the first time, and third time extracts 30min, each extraction time It is calculated after boiling, combined extract, the extracting solution of acquisition is concentrated to 3 that the extracting liquid volume is the raw material weight ~5 times, obtain initial concentration extracting solution；
Plus ethanol precipitation 2): add ethanol in proper amount into the initial concentration extracting solution of above-mentioned preparation, make solvent alcohol content 65~ 75%, 24 hours are stood, filtration, filtrate recycling ethanol obtains refined liquid, is concentrated, is drying to obtain " Magnoliae Powder side " traditional Chinese medicine extraction Object.
The macroporous resin purification preparation method of " 4. Magnoliae Powder side " Chinese medical extract, which is characterized in that with the flower bud of lily magnolia, asarum, rhizoma ligustici, Cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae and the root of Dahurain angelica are made of each equal part of raw material；Each raw material relative weight ratio is the flower bud of lily magnolia: thin It is pungent: rhizoma ligustici: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；
Preparation method includes the following steps:
1) it prepares concentrate: above-mentioned ingredients being cleaned, weighs raw material in proportion, 10~15 times of waters is added to impregnate 20- 30min heating extraction 3 times, extracts 1h, second of extraction 45min for the first time, and third time extracts 30min, each extraction time It is calculated after boiling, combined extract, the extracting solution of acquisition is concentrated to 3 that the extracting liquid volume is the raw material weight ~5 times, obtain initial concentration extracting solution；
2) macroporous resin purification: respectively plus in the initial concentration extracting solution that obtains to upper step of 3~5 times of volume hot water, supernatant is taken； Supernatant is crossed into macroporous resin column absorption, abandons efflux；Then it is washed with the water of 1~5BV with 0.5~2.5BV/ hours flow velocitys The adsorption column abandons water lotion；50~70% ethyl alcohol, 3~5BV of elution volume, with 0.5~2.5BV/ hours are used later Flow velocity elutes adsorption column, collects the ethanol eluate, and concentration, the dry ethanol eluate obtain " Magnoliae Powder side " Chinese medicine and mention Take object.
The macroporous resin purification preparation method of " 5. Magnoliae Powder side " Chinese medical extract, which is characterized in that with the flower bud of lily magnolia, asarum, rhizoma ligustici, Cimicifugae foetidae, Rhizoma Chuanxiong, caulis akebiae, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae and the root of Dahurain angelica are made of each equal part of raw material；Each raw material relative weight ratio is the flower bud of lily magnolia: thin It is pungent: rhizoma ligustici: cimicifugae foetidae: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；
Preparation method includes the following steps:
1) it prepares concentrate: taking each taste prepared slices of Chinese crude drugs, weigh raw material in proportion, 10~15 times of 65%~85% ethyl alcohol is added to impregnate 20-30min, heating and refluxing extraction 2 times, each 1h, the extracting solution of acquisition is concentrated to the volume of the extracting solution in combined extract It is 3~5 times of the raw material weight, obtains initial concentration extracting solution；
2) macroporous resin purification: respectively plus in the initial concentration extracting solution that obtains to upper step of 3~5 times of volume hot water, supernatant is taken； Supernatant is crossed into macroporous resin column absorption, abandons efflux；Adsorption column described in the water washing of 5BV is first used after loading, abandons water lotion；So The adsorption column was washed with 0.5~2.5BV/ hours flow velocitys with the water of 1~5BV afterwards, abandons water lotion；50~70% are used later Ethyl alcohol, 3~5BV of elution volume elutes adsorption column with 0.5~2.5BV/ hours flow velocitys, collects the ethanol eluate, dense Contracting, the dry ethanol eluate, obtain " Magnoliae Powder side " Chinese medical extract.
6. a kind of preparation method of " Magnoliae Powder side " powder: it is characterized in that, with the flower bud of lily magnolia, asarum, rhizoma ligustici, cimicifugae foetidae, Rhizoma Chuanxiong, wood Logical, radix saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae and the root of Dahurain angelica are made of each equal part of raw material；Each raw material relative weight ratio is the flower bud of lily magnolia: asarum: rhizoma ligustici: being risen Fiber crops: Rhizoma Chuanxiong: caulis akebiae: radix saposhnikoviae: Rhizoma Et Radix Notopterygii: Radix Glycyrrhizae: the root of Dahurain angelica=1:1:1:1:1:1:1:1:1:1；
Preparation method includes the following steps: to take each taste prepared slices of Chinese crude drugs, weighs raw material in proportion, finely ground mixing sieving is packed scattered Agent.
7. such as any one method is prepared in claim 1-5 " Magnoliae Powder side ", which is characterized in that in the extract By weight, magnelin is total not less than 0.04%, Notopterol and Isomperatorin not less than 0.22%, Imperatorin for amount Amount is not less than 0.22%.
8. containing the pharmaceutical composition such as any one method is prepared in claim 1-5 " Magnoliae Powder side ", feature It is, the composition is oral preparation, includes pharmaceutically acceptable carrier and/or figuration in the oral preparation Agent.
9. if " the Magnoliae Powder side " that any one method is prepared in claim 1-5 is in preparation treatment nasosinusitis and bronchitis Application in drug or health care product.
CN201810812353.XA 2018-07-23 2018-07-23 A kind of preparation method and applications of Chinese medical extract that treating nasosinusitis and bronchitis Pending CN109045120A (en)

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CN110585388A (en) * 2019-09-27 2019-12-20 赵升瑞 Oral liquid for stopping nasal discharge
CN116196251A (en) * 2023-05-06 2023-06-02 云南英格生物技术有限公司 Preparation method and application of notopterygium root extract

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110585388A (en) * 2019-09-27 2019-12-20 赵升瑞 Oral liquid for stopping nasal discharge
CN116196251A (en) * 2023-05-06 2023-06-02 云南英格生物技术有限公司 Preparation method and application of notopterygium root extract
CN116196251B (en) * 2023-05-06 2023-07-21 云南英格生物技术有限公司 Preparation method and application of notopterygium root extract

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