CN106511902A - Preparation method for traditional Chinese medicine preparation for relieving swelling and pain - Google Patents

Preparation method for traditional Chinese medicine preparation for relieving swelling and pain Download PDF

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Publication number
CN106511902A
CN106511902A CN201611157571.1A CN201611157571A CN106511902A CN 106511902 A CN106511902 A CN 106511902A CN 201611157571 A CN201611157571 A CN 201611157571A CN 106511902 A CN106511902 A CN 106511902A
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China
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parts
radix
preparation
chinese medicine
alleviating pain
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CN201611157571.1A
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韦飞燕
张艳华
刘春明
覃芳芳
方振
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GUANGXI HUAHONG PHARMACEUTICAL CO Ltd
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GUANGXI HUAHONG PHARMACEUTICAL CO Ltd
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00—Medicinal preparations containing organic active ingredients
    • A61K31/045—Hydroxy compounds, e.g. alcohols; Salts thereof, e.g. alcoholates
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00—Medicinal preparations containing organic active ingredients
    • A61K31/12—Ketones
    • A61K31/122—Ketones having the oxygen directly attached to a ring, e.g. quinones, vitamin K1, anthralin
    • A61K31/125—Camphor; Nuclear substituted derivatives thereof
    • 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)
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    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/21—Amaranthaceae (Amaranth family), e.g. pigweed, rockwort or globe amaranth
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    • A61K36/18—Magnoliophyta (angiosperms)
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    • A61K2236/10—Preparation or pretreatment of starting material
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    • A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
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Abstract

The invention discloses a preparation method for a traditional Chinese medicine preparation for relieving swelling and pain. The method comprises the following steps: taking 21 medicinal materials, including elecampane, radices sileris, schizonepeta, asarum, cortex acanthopanacis, cassia twigs, radix achyranthis bidentatae, ligusticum wallichii, cynanchum paniculatum, radix angelicae, curcuma zedoary, parabarium chunianum, ardisia quinquegona, dotted ardisia, radix zanthoxyli, herba fibraureae recisae, jasmine, rhizoma sparganii, agilawood, camphor and menthol; performing superfine smashing and ultrasonic treatment; and performing microwave extraction and micro-filtration, thereby acquiring the traditional Chinese medicine preparation. According to the invention, the ultrasonic technology is combined with the microwave extraction, so that the effective compositions of the medicinal materials are fully extracted, the loss is avoided, the pharmacological effect is increased, and the extraction time is shortened; grinding-resisting medicinal materials and easily-ground medicinal materials are separately treated, so that the pretreatment efficiency and extraction efficiency of the medicinal materials are increased; and an inorganic ceramic membrane separation technique is adopted for separating suspended particles from macromolecule impurities in the solution, the effective compositions are enriched, and the extraction efficiency is higher.

Description

A kind of preparation method of reducing swelling and alleviating pain Chinese medicine preparation
Technical field
A kind of a kind of the present invention relates to Chinese patent medicine preparation preparation method, more particularly to reducing swelling and alleviating pain with Chinese herbal medicine as raw material The preparation method of medicament.
Background technology
The preparation of Chinese medicine compound preparation is typically extracted using methods such as decocting method, circumfluence method, percolations, but have Extracting method temperature rising in extraction process easily causes thermal sensitivity effective ingredient and changes, and some extracting method are extracted Yield is low, extraction time is long.Due to the effective ingredient that Chinese crude drug complex chemical composition, traditional extraction process can be destroyed in medical material.
Repercussive and analgesic tincture for Guangxi Huahong Pharmaceutical Co., Ltd. exclusive product, the kind record in 《Chinese Pharmacopoeia》, product include 20 a herb raw materials, be related to the extraction of more medical materials.
And ultrasonic technology can increase molecular motion of material frequency and speed, increase solvent penetration power, improve medicine molten Go out speed and dissolution number of times, shorten extraction time, and Inorganic Ceramic Membranes are based on screening principle, in separable solution 0.05～10 μm of particle and some big molecular impurities.Chinese medicine separation inorganic ceramic film mostly is Al2O3Ceramic membrane, it has Have the advantages that stable chemical nature, high temperature resistant, pore-size distribution be narrow, high mechanical strength, it is active constituent-enriched, invalid impurity is removed, Extraction efficiency is higher, and effective ingredient has obtained effective protection, therefore, both approaches can be used as the group for improving medicinal material extract rate Conjunction method.
The present invention is that the improvement carried out on the basis of Chinese invention patent CN101099846A is invented, and the patent application is remembered The prescription and its preparation technology of this Chinese medicine composition is carried, the preparation technology is active constituent-enriched using the technique of percolation.
The content of the invention
It is an object of the invention to provide a kind of preparation method of reducing swelling and alleviating pain Chinese medicine preparation, protects active ingredients from traditional Chinese medicinal And improve extract yield.
For reaching object above, the present invention is adopted the technical scheme that：
A kind of preparation method of reducing swelling and alleviating pain Chinese medicine preparation, it is characterised in that including following preparation process：
Step 1, weighs the raw material of following weight portion：10～50 parts of the Radix Aucklandiae, 10～50 parts of Radix Saposhnikoviae, 10～50 parts of Herba Schizonepetae, carefully Pungent 10～50 parts, 10～50 parts of Cortex Acanthopanciss, 10～50 parts of Ramulus Cinnamomi, 10～50 parts of Radix Achyranthis Bidentatae, 10～50 parts of Rhizoma Chuanxiong, Radix Cynanchi Paniculati 10～50 Part, 20～50 parts of the Radix Angelicae Dahuricae, 10～50 parts of Rhizoma Curcumae, 20～50 parts of Radix seu Caulis Parabarii, 30～60 parts of DALUOSAN, 20～50 parts of Radix Ardisiae punctatae, two 30～60 parts of face pin, 25～60 parts of Caulis Fibraureae, 30～60 parts of Fructus Gardeniae, 20～50 parts of Rhizoma Sparganii, 5～60 parts of Lignum Aquilariae Resinatum, 16～50 parts of Camphora, 16～50 parts of Mentholum；
Step 2, is taken the 5 taste medical material such as the Radix Aucklandiae, Radix Saposhnikoviae, Rhizoma Chuanxiong, Rhizoma Sparganii, Lignum Aquilariae Resinatum, is carried out after wet ball grinding using ball mill, is used Ultrasonic grinding, then microwave extracting is carried out, combining extraction liquid, centrifugation collect supernatant；
Step 3, takes Herba Schizonepetae, Herba Asari, Cortex Acanthopanciss, Ramulus Cinnamomi, Radix Achyranthis Bidentatae, Radix Cynanchi Paniculati, the Radix Angelicae Dahuricae, Rhizoma Curcumae, DALUOSAN, Radix Ardisiae punctatae, red The 14 taste medical material such as the Cortex Eucommiae, Radix Zanthoxyli, Caulis Fibraureae, Fructus Gardeniae, using ball mill wet ball grinding, medicated powder extraction, combining extraction liquid are centrifuged, Collect supernatant；
Step 4, step 2 and the mixing of step 3 gained supernatant；
Step 5, carries out microfiltration using ceramic membrane to the solution obtained by step 4, collects filtrate；
Step 6, takes Camphora, Mentholum, is dissolved with ethanol in proper amount, mixes with step 5 gained filtrate.
Preferably, step 1 weighs the raw material of following parts by weight：47 parts of the Radix Aucklandiae, 47 parts of Radix Saposhnikoviae, 47 parts of Herba Schizonepetae, Herba Asari 47 parts, 47 parts of Cortex Acanthopanciss, 47 parts of Ramulus Cinnamomi, 47 parts of Radix Achyranthis Bidentatae, 47 parts of Rhizoma Chuanxiong, 47 parts of Radix Cynanchi Paniculati, 70 parts of the Radix Angelicae Dahuricae, 47 parts of Rhizoma Curcumae, red Du Secondary 70 parts, 50 parts of DALUOSAN, 40 parts of Radix Ardisiae punctatae, 50 parts of Radix Zanthoxyli, 50 parts of Caulis Fibraureae, 50 parts of Fructus Gardeniae, 30 parts of Rhizoma Sparganii, 50 parts of Lignum Aquilariae Resinatum, 40 parts of Camphora, 40 parts of Mentholum.
Preferably, 1.5～2h of Ball-milling Time described in step 2, ultrasonic frequency be 30～55KHz, power be 4000～ 6000W, 1.0～2.0h of ultrasonic treatment time, make the medicated powder that mesh number is 60～120 mesh.
Preferably, microwave extracting described in step 2, each time be 20～50min, microwave frequency be 3000～ 30000Hz, adds the ethanol solution that concentration of volume percent is 50～90% to be solvent, extracts 3～10 times, united extraction liquid, It is centrifuged with 1000～3000rpm of rotating speed.
Preferably, 0.2～0.5h of Ball-milling Time described in step 3, makes the medicated powder that mesh number is 60～120 mesh.
Preferably, extract described in step 3, add the ethanol solution that concentration of volume percent is 50～90% to be solvent, Extraction time is 20～50min every time, repeats extraction 3～10 times, and combining extraction liquid is centrifuged with 1000～3000rpm of rotating speed, is received Collection supernatant.
Preferably, the technological parameter of microfiltration described in step 5 is 0.3～0.5MPa of pressure, 1.5～2.5ml/s of flow velocity.
Preferably, the active component makes external preparation with conventional formulation means, such as gel, varnish, aerosol, Spray, unguentum.
Advantages of the present invention and effect：
1st, ultrasonic technology combines the mode of microwave extracting, effective ingredient is not destroyed, it is ensured that effective ingredient fills Foot, drug effect increase, and can also increase molecular motion of material frequency and speed, increase solvent penetration power in next step extraction step； Extracting process adopts microwave extracting, and during microwave extracting, frequency electromagnetic waves penetrate spe medium, and arrival is extracted the interior of material Portion, microwave energy are quickly converted to heat energy and make the temperature rapid increase of cell interior, when the pressure of cell interior exceedes cell During ability to bear, cell will rupture, and effective ingredient is i.e. from intracellular release, and is dissolved in spe medium, then by further It is separated by filtration, you can obtain extracted component.Ultrasonic technology can improve drug-eluting speed and dissolution number of times with reference to microwave extracting. Volatile component generally in medicine individually will be extracted, and using the extracting method of the present invention, can obtain volatile in medicine simultaneously Active substance, shorten more than half extraction time, reduce extraction step.
2nd, 5 taste medical materials of wear-resisting class sturdy to rhizome carry out ball milling and ultrasonic Treatment, and in addition 14 tastes are easily ground with medical material point Drive row ball milling into, the pretreatment efficiency and extraction efficiency of medical material can be improved.
3rd, using Inorganic Ceramic Membranes be based on screening principle, 0.05～10 μm of suspension in separable solution Grain and some big molecular impurities, it is active constituent-enriched, invalid impurity is removed, extraction efficiency is higher.
4th, percolation preparation time used by matched group is 72 hours, and preparation time of the present invention is within 10 hours, this Bright DNA purity is higher, and extraction time is shorter, the substantially high many of extraction efficiency.
Specific embodiment
Further is made to the reducing swelling and alleviating pain medicament preparation method described in the present invention and its application below by specific embodiment Explanation.It should be understood that embodiments of the invention are for illustrating rather than limitation of the present invention.According to this The substantial technological of invention belongs to the scope of protection of present invention to the simple modifications that the present invention is carried out.Second described in embodiment Determining alcohol is percent by volume.
Embodiment 1：
1. the raw material of following weight portion is weighed：Radix Aucklandiae 22g, Radix Saposhnikoviae 50g, Herba Schizonepetae 30g, Herba Asari 15g, Cortex Acanthopanciss 45g, Ramulus Cinnamomi 18g, Radix Achyranthis Bidentatae 70g, Rhizoma Chuanxiong 50g, Radix Cynanchi Paniculati 37g, Radix Angelicae Dahuricae 50g, Rhizoma Curcumae 36g, Radix seu Caulis Parabarii 48g, DALUOSAN 30g, Radix Ardisiae punctatae 20g, Radix Zanthoxyli 50g, Caulis Fibraureae 35g, Fructus Gardeniae 30g, Rhizoma Sparganii 50g, Lignum Aquilariae Resinatum 9g, Camphora 30g, Mentholum 50g.
2. the 5 taste medical material such as the Radix Aucklandiae, Radix Saposhnikoviae, Rhizoma Chuanxiong, Rhizoma Sparganii, Lignum Aquilariae Resinatum is taken, after coarse crushing, wet ball grinding is carried out using ball mill After 1.5h, ultrasonic grinding 1.0h is used, make the medicated powder that mesh number is 60 mesh, the ultrasonic frequency is 40KHz, power is 5000W, carries out microwave extracting 25min to medicated powder, so circulation 5 times, then extracting solution is positioned in centrifuge, in rotating speed 50min is centrifuged under conditions of 2000rpm, supernatant, ethanol solution of the extract for concentration 85% is collected, and microwave frequency is 3000Hz, collects supernatant.
3. take Herba Schizonepetae, Herba Asari, Cortex Acanthopanciss, Ramulus Cinnamomi, Radix Achyranthis Bidentatae, Radix Cynanchi Paniculati, the Radix Angelicae Dahuricae, Rhizoma Curcumae, DALUOSAN, Radix Ardisiae punctatae, Radix seu Caulis Parabarii, The 14 taste medical material such as Radix Zanthoxyli, Caulis Fibraureae, Fructus Gardeniae, after coarse crushing, carries out wet ball grinding 0.2h using ball mill, makes mesh number for 60 purposes Medicated powder, carries out extraction 25min using the ethanol solution of concentration 85% to medicated powder, so circulation 5 times, then by extracting solution be positioned over from In scheming, 50min is centrifuged under conditions of rotating speed 2000rpm, collect supernatant.
4. step 2 and step 3 gained supernatant are mixed.
5. microfiltration is carried out to the solution obtained by step 4 using ceramic membrane, the technological parameter of the microfiltration is：Pressure 0.4MPa, flow velocity 2.0m/s, collect filtrate.
6. take Camphora, Mentholum, with ethanol in proper amount dissolve, with above-mentioned filtrate mix be obtained active component, active component with Conventional formulation means make externally-used embrocation.
Embodiment 2：
1. the raw material of following weight portion is weighed：Radix Aucklandiae 10g, Radix Saposhnikoviae 10g, Herba Schizonepetae 10g, Herba Asari 10g, Cortex Acanthopanciss 10g, Ramulus Cinnamomi 10g, Radix Achyranthis Bidentatae 10g, Rhizoma Chuanxiong 10g, Radix Cynanchi Paniculati 10g, Radix Angelicae Dahuricae 20g, Rhizoma Curcumae 10g, Radix seu Caulis Parabarii 20g, DALUOSAN 30g, Radix Ardisiae punctatae 20g, Radix Zanthoxyli 30g, Caulis Fibraureae 25g, Fructus Gardeniae 30g, Rhizoma Sparganii 20g, Lignum Aquilariae Resinatum 5g, Camphora 16g, Mentholum 16g.
2. the 5 taste medical material such as the Radix Aucklandiae, Radix Saposhnikoviae, Rhizoma Chuanxiong, Rhizoma Sparganii, Lignum Aquilariae Resinatum is taken, after coarse crushing, wet ball grinding is carried out using ball mill After 1.8h, ultrasonic grinding 1.5h is used, make the medicated powder that mesh number is 80 mesh, the ultrasonic frequency is 30KHz, power is 4000W, carries out microwave extracting 20min to medicated powder, so circulation 3 times, then extracting solution is positioned in centrifuge, in rotating speed 1000 Under conditions of be centrifuged 30min, collect supernatant, ethanol solution of the extract for concentration 60%, microwave frequency is 8000Hz.
3. take Herba Schizonepetae, Herba Asari, Cortex Acanthopanciss, Ramulus Cinnamomi, Radix Achyranthis Bidentatae, Radix Cynanchi Paniculati, the Radix Angelicae Dahuricae, Rhizoma Curcumae, DALUOSAN, Radix Ardisiae punctatae, Radix seu Caulis Parabarii, The 14 taste medical material such as Radix Zanthoxyli, Caulis Fibraureae, Fructus Gardeniae, after coarse crushing, carries out wet ball grinding 0.3h using ball mill, makes mesh number for 80 purposes Medicated powder, carries out extraction 20min using the ethanol solution of concentration 60% to medicated powder, so circulation 3 times, then by extracting solution be positioned over from In scheming, 30min is centrifuged under conditions of rotating speed 1000rpm, collect supernatant.
4. step 2 and step 3 gained supernatant are mixed.
5. microfiltration is carried out to the upper solution obtained by step 3 using ceramic membrane, the technological parameter of the microfiltration is：Pressure 0.3MPa, flow velocity 1.5m/s, collect filtrate.
6. take Camphora, Mentholum, with ethanol in proper amount dissolve, with above-mentioned filtrate mix be obtained active component, active component with Conventional formulation means make externally used paste.
Embodiment 3：
1. the raw material of following weight portion is weighed：Radix Aucklandiae 50g, Radix Saposhnikoviae 50g, Herba Schizonepetae 50g, Herba Asari 50g, Cortex Acanthopanciss 50g, Ramulus Cinnamomi 50g, Radix Achyranthis Bidentatae 50g, Rhizoma Chuanxiong 50g, Radix Cynanchi Paniculati 50g, Radix Angelicae Dahuricae 50g, Rhizoma Curcumae 50g, Radix seu Caulis Parabarii 50g, DALUOSAN 60g, Radix Ardisiae punctatae 50g, Radix Zanthoxyli 60g, Caulis Fibraureae 60g, Fructus Gardeniae 60g, Rhizoma Sparganii 50g, Lignum Aquilariae Resinatum 60g, Camphora 50g, Mentholum 50g.
2. the sturdy wear-resisting medical material of the Radix Aucklandiae, Radix Saposhnikoviae, Rhizoma Chuanxiong, Rhizoma Sparganii, Lignum Aquilariae Resinatum rhizome is taken, after coarse crushing, is carried out using ball mill wet Method ball milling 1.9h, then ultrasound wave to crushing material process 2h, make the medicated powder that mesh number is 100 mesh, the ultrasonic frequency is 30KHz, power are 4000W, carry out microwave extracting 50min to medicated powder, so circulation 10 times, then extracting solution is positioned over centrifuge In, 60min is centrifuged under conditions of rotating speed 3000rpm, collects supernatant, the extract is the ethanol solution of concentration 95%, Microwave frequency is 10000Hz.
3. take Herba Schizonepetae, Herba Asari, Cortex Acanthopanciss, Ramulus Cinnamomi, Radix Achyranthis Bidentatae, Radix Cynanchi Paniculati, the Radix Angelicae Dahuricae, Rhizoma Curcumae, DALUOSAN, Radix Ardisiae punctatae, Radix seu Caulis Parabarii, Radix Zanthoxyli, Caulis Fibraureae, Fructus Gardeniae easily grind medical material, after coarse crushing, carry out wet ball grinding 0.4h using ball mill, make mesh number for 100 purposes Medicated powder, carries out extraction 50min using the ethanol solution of concentration 95% to medicated powder, so circulation 10 times, then extracting solution is positioned over In centrifuge, 60min is centrifuged under conditions of rotating speed 3000rpm, collect supernatant.
4. step 2 and step 3 gained supernatant are mixed.
5. microfiltration is carried out to the upper solution obtained by step 3 using ceramic membrane, the technological parameter of the microfiltration is：Pressure 0.5MPa, flow velocity 2.5m/s, collect filtrate.
6. taking Camphora, Mentholum and prepared active component being mixed with above-mentioned filtrate, active component is made with conventional formulation means Aerosol.
Embodiment 4：
1. the raw material of following weight portion is weighed：Radix Aucklandiae 50g, Radix Saposhnikoviae 40g, Herba Schizonepetae 50g, Herba Asari 10g, Cortex Acanthopanciss 50g, Ramulus Cinnamomi 10g, Radix Achyranthis Bidentatae 50g, Rhizoma Chuanxiong 50g, Radix Cynanchi Paniculati 50g, Radix Angelicae Dahuricae 45g, Rhizoma Curcumae 20g, Radix seu Caulis Parabarii 20g, DALUOSAN 30g, Radix Ardisiae punctatae 35g, Radix Zanthoxyli 60g, Caulis Fibraureae 25g, Fructus Gardeniae 50g, Rhizoma Sparganii 50g, Lignum Aquilariae Resinatum 55g, Camphora 26g, Mentholum 26g.
2. the sturdy wear-resisting medical material of the Radix Aucklandiae, Radix Saposhnikoviae, Rhizoma Chuanxiong, Rhizoma Sparganii, Lignum Aquilariae Resinatum rhizome is taken, after coarse crushing, is carried out using ball mill wet Method ball milling 2h, then ultrasound wave to crushing material process 1.8h, make the medicated powder that mesh number is 120 mesh, the ultrasonic frequency is 45KHz, power are 4800W, to medicated powder microwave extracting 25min, so circulation 6 times, then extracting solution is positioned in centrifuge, 40min is centrifuged under conditions of rotating speed 1800rpm, collects supernatant, ethanol solution of the extract for concentration 95%, Microwave Frequency Rate is 30000Hz.
3. take Herba Schizonepetae, Herba Asari, Cortex Acanthopanciss, Ramulus Cinnamomi, Radix Achyranthis Bidentatae, Radix Cynanchi Paniculati, the Radix Angelicae Dahuricae, Rhizoma Curcumae, DALUOSAN, Radix Ardisiae punctatae, Radix seu Caulis Parabarii, Radix Zanthoxyli, Caulis Fibraureae, Fructus Gardeniae easily grind medical material, after coarse crushing, carry out wet ball grinding 0.5h using ball mill, make mesh number for 120 purposes Medicated powder, carries out extraction 25min using the ethanol solution of concentration 95% to medicated powder, so circulation 6 times, then by extracting solution be positioned over from In scheming, 40min is centrifuged under conditions of rotating speed 1800rpm, collect supernatant.
4. step 2 and step 3 gained supernatant are mixed.
5. microfiltration is carried out to the upper solution obtained by step 3 using ceramic membrane, the technological parameter of the microfiltration is：Pressure 0.4MPa, flow velocity 2.0m/s, collect filtrate.
6. take Camphora, Mentholum and prepared active component is mixed with above-mentioned filtrate, make external spraying with conventional formulation means Agent.
Embodiment 5：
1. the raw material of following weight portion is weighed：Radix Aucklandiae 47g, Radix Saposhnikoviae 47g, Herba Schizonepetae 47g, Herba Asari 47g, Cortex Acanthopanciss 47g, Ramulus Cinnamomi 47g, Radix Achyranthis Bidentatae 47g, Rhizoma Chuanxiong 47g, Radix Cynanchi Paniculati 47g, Radix Angelicae Dahuricae 50g, Rhizoma Curcumae 47g, Radix seu Caulis Parabarii 50g, DALUOSAN 50g, Radix Ardisiae punctatae 40g, Radix Zanthoxyli 50g, Caulis Fibraureae 50g, Fructus Gardeniae 50g, Rhizoma Sparganii 30g, Lignum Aquilariae Resinatum 50g, Camphora 40g, Mentholum 40g.
2. the 5 taste medical material such as the Radix Aucklandiae, Radix Saposhnikoviae, Rhizoma Chuanxiong, Rhizoma Sparganii, Lignum Aquilariae Resinatum is taken, after coarse crushing, wet ball grinding 2h is carried out using ball mill Afterwards, ultrasonic grinding 1h is used, makes the medicated powder that mesh number is 120 mesh, the ultrasonic frequency for the ultrasonic frequency is 45KHz, power are 4800W, carry out microwave extracting 25min to the thin medicated powder of medicated powder, so circulation 6 times, then extracting solution is positioned over In centrifuge, 40min is centrifuged under conditions of rotating speed 1800rpm, collect supernatant, ethanol of the extract for concentration 75% Solution, microwave frequency are 20000Hz.
3. take Herba Schizonepetae, Herba Asari, Cortex Acanthopanciss, Ramulus Cinnamomi, Radix Achyranthis Bidentatae, Radix Cynanchi Paniculati, the Radix Angelicae Dahuricae, Rhizoma Curcumae, DALUOSAN, Radix Ardisiae punctatae, Radix seu Caulis Parabarii, The 14 taste medical material such as Radix Zanthoxyli, Caulis Fibraureae, Fructus Gardeniae, after coarse crushing, carries out wet ball grinding 0.4h using ball mill, makes mesh number for 120 mesh Medicated powder, extraction 25min is carried out to medicated powder using the ethanol solution of concentration 75%, so circulation 6 times, then extracting solution is positioned over In centrifuge, 40min is centrifuged under conditions of rotating speed 1800rpm, collect supernatant.
4. step 2 and step 3 gained supernatant are mixed.
5. microfiltration is carried out to the upper solution obtained by step 3 using ceramic membrane, the technological parameter of the microfiltration is：Pressure 0.5MPa, flow velocity 1.8m/s, collect filtrate.
6. taking Camphora, Mentholum and prepared active component being mixed with above-mentioned filtrate, active component is made with conventional formulation means Exterior-applied gel.
Matched group 1：Conventional percolation is extracted
1. Radix Aucklandiae 47g, Radix Saposhnikoviae 47g, Herba Schizonepetae 47g, Herba Asari 47g, Cortex Acanthopanciss 47g, Ramulus Cinnamomi 47g, Radix Achyranthis Bidentatae 47g, Rhizoma Chuanxiong 47g, Radix Cynanchi Paniculati 47g, Radix Angelicae Dahuricae 50g, Rhizoma Curcumae 47g, Radix seu Caulis Parabarii 50g, DALUOSAN 50g, Radix Ardisiae punctatae 40g, Radix Zanthoxyli 50g, Caulis Fibraureae 50g, Cape jasmine Sub- 50g, Rhizoma Sparganii 30g, Lignum Aquilariae Resinatum 50g, Camphora 40g, Mentholum 40g.
2. solvent is made with 53% ethanol, after 28 hours, slowly percolation, collects percolate to dipping；Camphora, Mentholum have mixed Full congruent melting, is mixed homogeneously with above-mentioned percolate and makes mixture of active principles.
Matched group 2：Remove ultrasonic grinding step
1. the raw material of following weight portion is weighed：Radix Aucklandiae 47g, Radix Saposhnikoviae 47g, Herba Schizonepetae 47g, Herba Asari 47g, Cortex Acanthopanciss 47g, Ramulus Cinnamomi 47g, Radix Achyranthis Bidentatae 47g, Rhizoma Chuanxiong 47g, Radix Cynanchi Paniculati 47g, Radix Angelicae Dahuricae 50g, Rhizoma Curcumae 47g, Radix seu Caulis Parabarii 50g, DALUOSAN 50g, Radix Ardisiae punctatae 40g, Radix Zanthoxyli 50g, Caulis Fibraureae 50g, Fructus Gardeniae 50g, Rhizoma Sparganii 30g, Lignum Aquilariae Resinatum 50g, Camphora 40g, Mentholum 40g.
2. the sturdy wear-resisting medical material of the Radix Aucklandiae, Radix Saposhnikoviae, Rhizoma Chuanxiong, Rhizoma Sparganii, Lignum Aquilariae Resinatum rhizome is taken, after coarse crushing, is carried out using ball mill wet Method ball milling 2h, makes the medicated powder that mesh number is 120 mesh, carries out microwave extracting 25min to the thin medicated powder of medicated powder, so circulation 6 times, then will Extracting solution is positioned in centrifuge, and 40min is centrifuged under conditions of rotating speed 1800rpm, collects supernatant, and the extract is dense The ethanol solution of degree 75%, microwave frequency is 20000Hz.
3. take Herba Schizonepetae, Herba Asari, Cortex Acanthopanciss, Ramulus Cinnamomi, Radix Achyranthis Bidentatae, Radix Cynanchi Paniculati, the Radix Angelicae Dahuricae, Rhizoma Curcumae, DALUOSAN, Radix Ardisiae punctatae, Radix seu Caulis Parabarii, Radix Zanthoxyli, Caulis Fibraureae, Fructus Gardeniae easily grind medical material, after coarse crushing, carry out wet ball grinding 0.4h using ball mill, make mesh number for 120 purposes Medicated powder, carries out extraction 25min using the ethanol solution of concentration 75% to medicated powder, so circulation 6 times, then by extracting solution be positioned over from In scheming, 40min is centrifuged under conditions of rotating speed 1800rpm, collect supernatant.
4. step 2 and step 3 gained supernatant are mixed.
5. microfiltration is carried out to the upper solution obtained by step 3 using ceramic membrane, the technological parameter of the microfiltration is：Pressure 0.5MPa, flow velocity 1.8m/s, collect filtrate.
6. taking Camphora, Mentholum and prepared active component being mixed with above-mentioned filtrate, active component is made with conventional formulation means Exterior-applied gel.
Matched group 3：Microwave extracting is changed to ethanol solution conventional extraction
1. the raw material of following weight portion is weighed：Radix Aucklandiae 47g, Radix Saposhnikoviae 47g, Herba Schizonepetae 47g, Herba Asari 47g, Cortex Acanthopanciss 47g, Ramulus Cinnamomi 47g, Radix Achyranthis Bidentatae 47g, Rhizoma Chuanxiong 47g, Radix Cynanchi Paniculati 47g, Radix Angelicae Dahuricae 50g, Rhizoma Curcumae 47g, Radix seu Caulis Parabarii 50g, DALUOSAN 50g, Radix Ardisiae punctatae 40g, Radix Zanthoxyli 50g, Caulis Fibraureae 50g, Fructus Gardeniae 50g, Rhizoma Sparganii 30g, Lignum Aquilariae Resinatum 50g, Camphora 40g, Mentholum 40g.
2. the sturdy wear-resisting medical material of the Radix Aucklandiae, Radix Saposhnikoviae, Rhizoma Chuanxiong, Rhizoma Sparganii, Lignum Aquilariae Resinatum rhizome is taken, after coarse crushing, is carried out using ball mill wet Method ball milling 2h, then ultrasound wave to crushing material process 1.8h, make the medicated powder that mesh number is 120 mesh, the ultrasonic frequency is 45KHz, power are 4800W, extract 25min, so circulation 6 times to medicated powder using the ethanol solution of concentration 95%, then will extract Liquid is positioned in centrifuge, and 40min is centrifuged under conditions of rotating speed 1800rpm, collects supernatant.
3. take Herba Schizonepetae, Herba Asari, Cortex Acanthopanciss, Ramulus Cinnamomi, Radix Achyranthis Bidentatae, Radix Cynanchi Paniculati, the Radix Angelicae Dahuricae, Rhizoma Curcumae, DALUOSAN, Radix Ardisiae punctatae, Radix seu Caulis Parabarii, Radix Zanthoxyli, Caulis Fibraureae, Fructus Gardeniae easily grind medical material, after coarse crushing, carry out wet ball grinding 0.5h using ball mill, make mesh number for 120 purposes Medicated powder, carries out extraction 25min using the ethanol solution of concentration 95% to medicated powder, so circulation 6 times, then by extracting solution be positioned over from In scheming, 40min is centrifuged under conditions of rotating speed 1800rpm, collect supernatant.
4. step 2 and step 3 gained supernatant are mixed.
5. microfiltration is carried out to the upper solution obtained by step 3 using ceramic membrane, the technological parameter of the microfiltration is：Pressure 0.4MPa, flow velocity 2.0m/s, collect filtrate.
6. take Camphora, Mentholum and prepared active component is mixed with above-mentioned filtrate, make external spraying with conventional formulation means Agent.
Matched group 4：All medical materials are processed simultaneously
1. the raw material of following weight portion is weighed：Radix Aucklandiae 47g, Radix Saposhnikoviae 47g, Herba Schizonepetae 47g, Herba Asari 47g, Cortex Acanthopanciss 47g, Ramulus Cinnamomi 47g, Radix Achyranthis Bidentatae 47g, Rhizoma Chuanxiong 47g, Radix Cynanchi Paniculati 47g, Radix Angelicae Dahuricae 50g, Rhizoma Curcumae 47g, Radix seu Caulis Parabarii 50g, DALUOSAN 50g, Radix Ardisiae punctatae 40g, Radix Zanthoxyli 50g, Caulis Fibraureae 50g, Fructus Gardeniae 50g, Rhizoma Sparganii 30g, Lignum Aquilariae Resinatum 50g.
2. after above-mentioned raw materials coarse crushing, wet ball grinding 2h is carried out using ball mill, then ultrasound wave is to crushing material process 1.8h, makes the medicated powder that mesh number is 120 mesh, and the ultrasonic frequency is 45KHz, and power is 4800W.
3. thin medicated powder carries out microwave extracting 25min, so circulation 6 times, then extracting solution is positioned in centrifuge, in rotating speed 40min is centrifuged under conditions of 1800rpm, collects supernatant, ethanol solution of the extract for concentration 75%.
4. microfiltration is carried out to the upper solution obtained by step 3 using ceramic membrane, the technological parameter of the microfiltration is：Pressure 0.5MPa, flow velocity 1.8m/s, collect filtrate.
5. taking Camphora 40g, Mentholum 40g and prepared active component being mixed with above-mentioned filtrate, active component is with conventional formulation handss Section makes exterior-applied gel.
Matched group 5：Remove ceramic membrane filter step
1. the raw material of following weight portion is weighed：Radix Aucklandiae 47g, Radix Saposhnikoviae 47g, Herba Schizonepetae 47g, Herba Asari 47g, Cortex Acanthopanciss 47g, Ramulus Cinnamomi 47g, Radix Achyranthis Bidentatae 47g, Rhizoma Chuanxiong 47g, Radix Cynanchi Paniculati 47g, Radix Angelicae Dahuricae 50g, Rhizoma Curcumae 47g, Radix seu Caulis Parabarii 50g, DALUOSAN 50g, Radix Ardisiae punctatae 40g, Radix Zanthoxyli 50g, Caulis Fibraureae 50g, Fructus Gardeniae 50g, Rhizoma Sparganii 30g, Lignum Aquilariae Resinatum 50g, Camphora 40g, Mentholum 40g.
2. the sturdy wear-resisting medical material of the Radix Aucklandiae, Radix Saposhnikoviae, Rhizoma Chuanxiong, Rhizoma Sparganii, Lignum Aquilariae Resinatum rhizome is taken, after coarse crushing, is carried out using ball mill wet Method ball milling 2h, then ultrasound wave to crushing material process 1.8h, make the medicated powder that mesh number is 120 mesh, the ultrasonic frequency is 45KHz, power are 4800W, extract 25min, so circulation 6 times to medicated powder using the ethanol solution of concentration 95%, then will extract Liquid is positioned in centrifuge, and 40min is centrifuged under conditions of rotating speed 1800rpm, collects supernatant.
3. take Herba Schizonepetae, Herba Asari, Cortex Acanthopanciss, Ramulus Cinnamomi, Radix Achyranthis Bidentatae, Radix Cynanchi Paniculati, the Radix Angelicae Dahuricae, Rhizoma Curcumae, DALUOSAN, Radix Ardisiae punctatae, Radix seu Caulis Parabarii, Radix Zanthoxyli, Caulis Fibraureae, Fructus Gardeniae easily grind medical material, after coarse crushing, carry out wet ball grinding 0.5h using ball mill, make mesh number for 120 purposes Medicated powder, carries out extraction 25min using the ethanol solution of concentration 95% to medicated powder, so circulation 6 times, then by extracting solution be positioned over from In scheming, 40min is centrifuged under conditions of rotating speed 1800rpm, collect supernatant.
4. step 2 and step 3 gained supernatant are mixed.
5. take Camphora, Mentholum and step 4 gained supernatant and mix prepared active component, made with conventional formulation means outer Use spray.
Experimental example 1：
The change feelings for extracting soluble solid content in medicinal liquid before and after ceramic membrane filtration can be measured by compound microcapsule Condition.Its principle is to treat the index of refraction of sample measuring liquid at 20 DEG C with refractometer measurement, and with index of refraction and soluble solid content Conversion table is checked in or directly reads soluble solid content from refractometer.
Concrete operation method is as follows：
1. correction refractometer before determining.
2. separate refractometer two sides prism, ethanol is dipped in absorbent cotton and cleaned.
3. the drop of the sample 2～3 after ceramic membrane before processing is dipped with the Glass rod of the molten circle in end, drip in refractometer prism facets Centre.
4. rapid closing prism, stands about 1min, makes sample uniform bubble-free, and is full of the visual field.
5. alignment light source, observes objective lenses by eyepiece.Adjust and indicate rule, make the visual field be divided into light and shade two parts, then rotate Screw, makes terminator clear, and makes its demarcation line just on the decussation point of objective lenses.Read in the eyepiece visual field Percent or index of refraction, and record prism temperature.
6. eye piece reading scale is index of refraction, can be scaled soluble solid percentage composition by annex, as shown in table 1.
1 soluble solid of table removes test (%)
As shown in Table 1, the soluble solid clearance of embodiment products obtained therefrom is 25.4%～27.0%, inorganic ceramic In membrance separation solution, particle and some big molecular impurities, active constituent-enriched.
Experimental example 2 (accelerated stability experiment)
Take the medicament of the present invention prepared according to embodiment 1 to be incorporated with lid scale test tube and have in lid centrifuge tube, be placed in temperature Spend for 38 DEG C ± 2 DEG C, relative humidity is to place 6 months under conditions of 55% ± 5%, is sampled respectively at the 0th, 1,2,3,6 months, After being mixed with the rotating speed centrifugation 15min of 4000r/min, 3h is stood, settling volume percentage ratio is observed, as shown in table 2.
Table 2 counts efficacy experiment
As shown in Table 2, medicament of the present invention is 38 DEG C ± 2 DEG C in temperature, and relative humidity is placement under conditions of 55% ± 5% 6 months, settling volume percentage ratio remained to maintain less than 5%, and lamination is not obvious, illustrated its good stability, and matched group 1 With the settling volume percentage ratio of matched group 5 up to more than 15%, its stability difference more of the present invention is illustrated.
Experimental example 3：Acute jerk contused wound therapeutic effect is observed
Experimental group：Embodiment 1～5 prepares gained sample.
Matched group：Above-mentioned matched group 1～4 prepares gained sample.
300 acute jerk contused wound patients are chosen, the age is between 30～50 years old.Above-mentioned 300 patients are randomly divided into into 6 Group, 50 per group, wherein 3 groups use control sample, and 3 groups use experimental example sample, are used in conjunction 5 days, observation and treatment effect.
Efficacy assessment standard：
Recovery from illness：Pain relief in medication 1 day, swelling in 2 days start to mitigate, disappearance of swelling and ache in 3 days, and joint function recovery is just Often；
It is effective：Pain relief in medication 1 day, swelling in 2 days start to mitigate, disappearance of swelling and ache in 5 days, and joint function recovery is just Often；
Effectively：Pain relief in medication 1 day, swelling in 2 days start to mitigate, and swell and ache in 5 days, and function of joint shows Writing improves；
It is invalid：Above-mentioned standard person is not reached.
Statistics curative effect such as table 3.
Table 3 counts efficacy experiment
Numbering Recovery from illness It is effective Effectively It is invalid Cure-remarkable-effectiveness rate
Embodiment 1 12 19 18 1 62.00%
Embodiment 2 11 21 16 2 66.00%
Embodiment 3 10 22 18 0 64.00%
Embodiment 4 9 23 15 3 64.00%
Embodiment 5 11 22 16 1 66.00%
Matched group 1 10 16 20 4 52.00%
Matched group 2 10 17 20 4 54.00%
Matched group 3 9 17 19 6 50.00%
Matched group 4 11 20 18 1 62.00%
As can be seen from Table 2,1～5 curative effect of embodiment is better than matched group, i.e., made by painting this method, medicament is anxious in treatment Property bruise curative effect be better than matched group, illustrate reducing swelling and alleviating pain agent prepared according to the methods of the invention with matched group same dose In the case of, the effective ingredient for treating acute jerk contused wound is significantly larger than matched group.Compared with matched group 1, which extracts embodiment 1～5 Time is short, and curative effect is better than matched group, and percolation preparation time used by matched group is 72 hours, and preparation time of the present invention is little 10 When within, DNA purity of the present invention is higher, and extraction time is shorter, the substantially high many of extraction efficiency；Embodiment 1～5 with compare Group 2 is compared, and be increased ultrasonic grinding material step, effective ingredient is not destroyed, it is ensured that effective ingredient is sufficient, may be used also To increase molecular motion of material frequency and speed, increase solvent penetration power in next step extraction step, curative effect is better than matched group 2； Compared with matched group 3, its extracting process adopts microwave extracting to embodiment 1～5, can improve drug-eluting speed and dissolution number of times, In medicine volatile active substance is collected simultaneously can, curative effect is better than matched group 3；Embodiment 1～5 compared with matched group 4, this Bright separately to be processed using wear-resisting medical material and easily mill medical material, matched group 4 is processed medical material used simultaneously, on the close basis of curative effect On, present invention saves the energy consumption of ball milling, microwave extracting and ultrasonic Treatment.
Although above having used general explanation, specific embodiment and test, the present invention having been made to retouch in detail State, but on the basis of the present invention, it can be made some modifications or improvements, this is apparent to those skilled in the art 's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed Scope.

Claims (9)

1. a kind of preparation method of reducing swelling and alleviating pain Chinese medicine preparation, it is characterised in that including following preparation process：
Step 1, weighs the raw material of following parts by weight：10～50 parts of the Radix Aucklandiae, 10～50 parts of Radix Saposhnikoviae, 10～50 parts of Herba Schizonepetae, Herba Asari 10～50 parts, 10～50 parts of Cortex Acanthopanciss, 10～50 parts of Ramulus Cinnamomi, 10～50 parts of Radix Achyranthis Bidentatae, 10～50 parts of Rhizoma Chuanxiong, Radix Cynanchi Paniculati 10～50 Part, 20～50 parts of the Radix Angelicae Dahuricae, 10～50 parts of Rhizoma Curcumae, 20～50 parts of Radix seu Caulis Parabarii, 30～60 parts of DALUOSAN, 20～50 parts of Radix Ardisiae punctatae, two 30～60 parts of face pin, 25～60 parts of Caulis Fibraureae, 30～60 parts of Fructus Gardeniae, 20～50 parts of Rhizoma Sparganii, 5～60 parts of Lignum Aquilariae Resinatum, 16～50 parts of Camphora, 16～50 parts of Mentholum；
Step 2, is taken the 5 taste medical material such as the Radix Aucklandiae, Radix Saposhnikoviae, Rhizoma Chuanxiong, Rhizoma Sparganii, Lignum Aquilariae Resinatum, is carried out after wet ball grinding using ball mill, with ultrasound Ripple is crushed, then carries out microwave extracting, combining extraction liquid, centrifugation, collects supernatant；
Step 3, take Herba Schizonepetae, Herba Asari, Cortex Acanthopanciss, Ramulus Cinnamomi, Radix Achyranthis Bidentatae, Radix Cynanchi Paniculati, the Radix Angelicae Dahuricae, Rhizoma Curcumae, DALUOSAN, Radix Ardisiae punctatae, Radix seu Caulis Parabarii, The 14 taste medical material such as Radix Zanthoxyli, Caulis Fibraureae, Fructus Gardeniae, using ball mill wet ball grinding, medicated powder extraction, combining extraction liquid, centrifugation, in collection Clear liquid；
Step 4, takes step 2 and step 3 gained supernatant, mixing；
Step 5, carries out microfiltration using ceramic membrane to the solution obtained by step 4, collects filtrate；
Step 6, takes Camphora, Mentholum, is dissolved with ethanol in proper amount, mixes with step 5 gained filtrate.
2. the preparation method of reducing swelling and alleviating pain Chinese medicine preparation as claimed in claim 1, it is characterised in that：Step 1 weighs following weight The raw material of number：47 parts of the Radix Aucklandiae, 47 parts of Radix Saposhnikoviae, 47 parts of Herba Schizonepetae, 47 parts of Herba Asari, 47 parts of Cortex Acanthopanciss, 47 parts of Ramulus Cinnamomi, 47 parts of Radix Achyranthis Bidentatae, river 47 parts of rhizome of chuanxiong, 47 parts of Radix Cynanchi Paniculati, 50 parts of the Radix Angelicae Dahuricae, 47 parts of Rhizoma Curcumae, 50 parts of Radix seu Caulis Parabarii, 50 parts of DALUOSAN, 40 parts of Radix Ardisiae punctatae, Radix Zanthoxyli 50 Part, 50 parts of Caulis Fibraureae, 50 parts of Fructus Gardeniae, 30 parts of Rhizoma Sparganii, 50 parts of Lignum Aquilariae Resinatum, 40 parts of Camphora, 40 parts of Mentholum.
3. the preparation method of reducing swelling and alleviating pain Chinese medicine preparation as claimed in claim 1, it is characterised in that：Ball-milling Time described in step 2 1.5～2h, ultrasonic frequency are 30～55KHz, and power is 4000～6000W, 1.0～2.0h of ultrasonic treatment time, is made Mesh number is the medicated powder of 60～120 mesh.
4. the preparation method of reducing swelling and alleviating pain Chinese medicine preparation as claimed in claim 1, it is characterised in that：Microwave extracting described in step 2, Time is 20～50min every time, and microwave frequency is 3000～30000Hz, adds the second that concentration of volume percent is 50～90% Alcoholic solution is solvent, is extracted 3～10 times, united extraction liquid, is centrifuged with 1000～3000rpm of rotating speed.
5. the preparation method of reducing swelling and alleviating pain Chinese medicine preparation as claimed in claim 1, it is characterised in that：Ball-milling Time described in step 3 0.2～0.5h, makes the medicated powder that mesh number is 60～120 mesh.
6. the preparation method of reducing swelling and alleviating pain Chinese medicine preparation as claimed in claim 1, it is characterised in that：Extract described in step 3, add Concentration of volume percent be 50～90% ethanol solution be solvent, each extraction time be 20～50min, repeat extraction 3～ 10 times, combining extraction liquid is centrifuged with 1000～3000rpm of rotating speed, collects supernatant.
7. the preparation method of reducing swelling and alleviating pain Chinese medicine preparation as claimed in claim 1, it is characterised in that：Microfiltration described in step 5, pressure For 0.3～0.8MPa, flow velocity is 1.5～2.5ml/s.
8. preparation obtained by the preparation method of reducing swelling and alleviating pain Chinese medicine composition according to any one of claim 1-7, its feature exist In：Said preparation by described in any one of claim 1-7 reducing swelling and alleviating pain Chinese medicine composition with the separately made gel of conventional formulation means Agent, varnish, aerosol, spray, the one of which of unguentum.
9. preparation obtained by the preparation method of reducing swelling and alleviating pain Chinese medicine composition according to any one of claim 1-7, its feature exist In：Said preparation reducing swelling and alleviating pain Chinese medicine composition and pharmaceutically acceptable carrier described in any one of claim 1-7 are constituted, with Conventional formulation means make the one of which of gel, varnish, aerosol, spray, unguentum.
CN201611157571.1A 2016-12-15 2016-12-15 Preparation method for traditional Chinese medicine preparation for relieving swelling and pain Withdrawn CN106511902A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115463181A (en) * 2021-06-10 2022-12-13 长沙学院 Preparation method of agilawood leaf extract

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115463181A (en) * 2021-06-10 2022-12-13 长沙学院 Preparation method of agilawood leaf extract
CN115463181B (en) * 2021-06-10 2024-01-30 长沙学院 Preparation method of agilawood leaf extract

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Application publication date: 20170322