CN109528795A - A kind of hempleaf groundsel herb granule and preparation method thereof - Google Patents

A kind of hempleaf groundsel herb granule and preparation method thereof Download PDF

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CN109528795A
CN109528795A CN201811508564.0A CN201811508564A CN109528795A CN 109528795 A CN109528795 A CN 109528795A CN 201811508564 A CN201811508564 A CN 201811508564A CN 109528795 A CN109528795 A CN 109528795A
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groundsel herb
hempleaf groundsel
granule
hempleaf
obtains
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廖年生
胡贤德
眭荣春
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Jiangxi Gan Long Pharmaceutical Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/28Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605Excipients; Inactive ingredients
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61P7/00Drugs for disorders of the blood or the extracellular fluid
    • A61P7/04Antihaemorrhagics; Procoagulants; Haemostatic agents; Antifibrinolytic agents
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K2236/30Extraction of the material
    • A61K2236/39Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

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Abstract

The present invention relates to Chinese medicinal granule technical field, a kind of hempleaf groundsel herb granule and preparation method thereof is disclosed.Method includes the following steps: (1) dries hempleaf groundsel herb rhizome, crush, obtains the particle that granularity is 40-100 mesh;(2) particulate matter that step (1) obtains is mixed with ethanol water, wherein by volume, the inventory of ethanol water is 10-15 times of the particulate matter inventory;(3) ultrasonic extraction 2-3 times;(4) it filters, gained filtrate decompression is concentrated;(5) gained concentrate is mixed with pharmaceutically acceptable auxiliary material, is freeze-dried, collected dried cream powder, crushed 80 meshes, be placed in mixing channel mixing, obtain hempleaf groundsel herb paste;(6) gained hempleaf groundsel herb paste is pelletized, particle successively uses 20 meshes and 50 mesh sieves, obtains hempleaf groundsel herb granule.The hempleaf groundsel herb granule active component content with higher prepared using method of the present invention, and particle size uniformity.

Description

A kind of hempleaf groundsel herb granule and preparation method thereof
Technical field
The present invention relates to Chinese medicinal granule technical fields, and in particular to a kind of hempleaf groundsel herb granule and its preparation side Method.
Background technique
Chinese medicinal granule is using traditional Chinese medicine medicine materical crude slice as raw material, by modern processing technique and pharmaceutical technology to medicinal material Full ingredient the processing such as extract, separate, be concentrated, dry, pelletize and pack and obtain, without decocting, for be directly formulated with The granule taken after mixing it with water.Chinese medicinal granule not only remained the effective component of the prepared slices of Chinese crude drugs, cures mainly and effect, but also had standard system One, curative effect is stable, easy to carry and do not have the advantages of of medicine materical crude slice such as be easy to adjust, and is taken after mixing it with water, can be made with granule composition prescription For the supplement of traditional Chinese herbal decoction and Chinese patent drug.
Hempleaf groundsel herb is perennial herb, is mainly distributed on Northeast China, northwest, North China.The root and rhizome of hempleaf groundsel herb Chinese medicine can be entered, main active is isoquercitrin, hempleaf groundsel herb glucoside, grass polysaccharide of returning from the grave etc..It can be used for treating abundant expectoration, asthma, It coughs up phlegm a variety of diseases such as not well, overstrain cough hemoptysis, there is very high medical value.However, there is presently no about hempleaf groundsel herb formula The report of particle and its preparation process.
Summary of the invention
The purpose of the invention is to provide a kind of hempleaf groundsel herb granule and preparation method thereof.
The present invention provides a kind of preparation methods of hempleaf groundsel herb granule, comprising the following steps:
(1) hempleaf groundsel herb rhizome is dried, is crushed, obtain the particle that granularity is 40-100 mesh;
(2) particulate matter that step (1) obtains is mixed with ethanol water, wherein by volume, the throwing of ethanol water Doses is 10-15 times of the particulate matter inventory;
(3) ultrasonic extraction 2-3 times;
(4) it filters, gained filtrate decompression is concentrated to the concentrate that relative density is 1.1-1.2;
(5) concentrate that step (4) obtains is mixed with pharmaceutically acceptable auxiliary material, is freeze-dried, collected dry Cream powder crushed 80 meshes, is placed in mixing channel mixing, obtains hempleaf groundsel herb paste;
(6) the hempleaf groundsel herb paste for obtaining step (5) is pelletized, and particle is successively used 20 meshes and 50 mesh sieves, returned Soul grass granule.
The present invention also provides the hempleaf groundsel herb granules prepared by the above method.
It according to the method described in the present invention, can (such as isoquercitrin be returned from the grave by the main active in hempleaf groundsel herb medicinal material Careless glucoside, grass polysaccharide of returning from the grave) sufficiently extract, the active substances such as plant fiber can be effectively removed, the steady of drug is improved It is qualitative, easy to store, is convenient to take.Moreover, the grain forming of the hempleaf groundsel herb granule prepared according to the method described in the present invention Preferably, particle size uniformity.In addition, directly being prepared using hempleaf groundsel herb medicinal material as raw material in method of the present invention, implement It is convenient, industrialization easy to accomplish.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more New numberical range, these numberical ranges should be considered as specific open herein.
The preparation method of hempleaf groundsel herb granule of the present invention the following steps are included:
(1) hempleaf groundsel herb rhizome is dried, is crushed, obtain the particle that granularity is 40-100 mesh;
(2) particulate matter that step (1) obtains is mixed with ethanol water, wherein by volume, the throwing of ethanol water Doses is 10-15 times of the particulate matter inventory;
(3) ultrasonic extraction 2-3 times;
(4) it filters, gained filtrate decompression is concentrated to the concentrate that relative density is 1.1-1.2;
(5) concentrate that step (4) obtains is mixed with pharmaceutically acceptable auxiliary material, is freeze-dried, collected dry Cream powder crushed 80 meshes, is placed in mixing channel mixing, obtains hempleaf groundsel herb paste;
(6) the hempleaf groundsel herb paste for obtaining step (5) is pelletized, and particle is successively used 20 meshes and 50 mesh sieves, returned Soul grass granule.
In method of the present invention, by volume, the inventory of the ethanol water is that the particulate matter feeds intake 10-15 times of amount specifically, such as can be 10 times, 11 times, 12 times, 13 times, 14 times or 15 times.In side of the present invention In method, hempleaf groundsel herb medicinal material is made to feed intake with the ethanol water according to such volume ratio, can sufficiently extracted described Main active in hempleaf groundsel herb medicinal material.
In method of the present invention, the temperature that hempleaf groundsel herb rhizome is dried can be 50-65 DEG C, and the time can be 1- 10 hours.
In method of the present invention, it is preferable that hempleaf groundsel herb rhizome is ground into the powdery that granularity is 40-100 mesh, is made Active constituent in hempleaf groundsel herb rhizome can rapidly extracting come out.
In method of the present invention, it is preferable that the ultrasonic frequency used during ultrasonic extraction is 50- 125kHz, each extraction time are 30-60 minutes.In method of the present invention, make hempleaf groundsel herb in the ethanol water The time of middle ultrasonic extraction and frequency can sufficiently extract the main active in hempleaf groundsel herb within above range, and And active constituent can be prevented to be denaturalized, so that the hempleaf groundsel herb granule of preparation has preferable drug effect.
In method of the present invention, the concentration of the ethanol water is 40-60 weight %, preferably 45-55 weight Measure %.
In method of the present invention, filtering can use the strainer filtering of this field routine.In specific embodiment party In formula, the strainer can be the stainless steel cloth that mesh size is 200 mesh.
In method of the present invention, it is preferable that the auxiliary material is soluble starch, starch, lactose, sucrose and dextrin At least one of.It is further preferred that the auxiliary material is the mixing of starch, lactose and dextrin.When the auxiliary material is starch, cream When the mixing of sugar and dextrin, the mixed weight ratio of three is preferably 1:0.01-0.5:0.1-2.
In method of the present invention, the feeding quantity of the auxiliary material makes the specification of hempleaf groundsel herb granule be every 1-3 Gram it is equivalent to 6-18 grams of hempleaf groundsel herb medicinal material.
In method of the present invention, the method for the granulation can be to make the hempleaf groundsel herb paste sieving Grain.
In method of the present invention, by making the particle obtained after granulation successively use 20 meshes and 50 mesh sieves, The hempleaf groundsel herb granule of particle size uniformity can be obtained.
The present invention also provides the hempleaf groundsel herb granules prepared by the above method.
Preferably, the specification of the hempleaf groundsel herb granule is equivalent to 6-18 grams of hempleaf groundsel herb medicinal material for every 1-3 grams, specifically Ground, every 1 gram of hempleaf groundsel herb granule are equivalent to 6 grams of hempleaf groundsel herb raw medicinal herbs, and every 2 grams of hempleaf groundsel herb granules are equivalent to 12 grams of hempleaf groundsel herb raw medicinal herbs, every 3 grams of hempleaf groundsel herb granules are equivalent to 18 grams of hempleaf groundsel herb raw medicinal herbs.
The present invention will be described in detail by way of examples below.
Embodiment 1
1kg hempleaf groundsel herb rhizome is taken, 5 hours dry at 60 DEG C, being crushed to granularity is 80 mesh, adds 13 times of inventory of ethyl alcohol Aqueous solution (concentration is 50 weight %), ultrasonic extraction 3 times under the ultrasonic frequency of 90kHz are extracted 45 minutes, every time with 200 Purpose stainless steel wire net filtration, filtrate decompression are concentrated to the concentrate that relative density is 1.15.100g is added in concentrate to form sediment The mixture (three's weight ratio is 1:0.25:1) of powder, lactose and dextrin mixes, and is freeze-dried, collects dried cream powder, crushes 80 meshes are crossed, mixing channel mixing is set.Hempleaf groundsel herb paste, sieving granulation are taken, particle is successively used 20 meshes and 50 mesh sieves, must be returned Soul grass granule sample A1.
Embodiment 2
1kg hempleaf groundsel herb rhizome is taken, 10 hours dry at 50 DEG C, being crushed to granularity is 100 mesh, adds 10 times of inventory of second Alcohol solution (concentration is 58 weight %), ultrasonic extraction 3 times under the ultrasonic frequency of 90kHz are extracted 45 minutes every time, are used The stainless steel wire net filtration of 200 mesh, filtrate decompression are concentrated to the concentrate that relative density is 1.12.100g is added in concentrate The mixture (three's weight ratio is 1:0.4:0.6) of starch, lactose and dextrin mixes, and is freeze-dried, collects dried cream powder, powder Broken 80 mesh of mistake sets mixing channel mixing.Hempleaf groundsel herb paste, sieving granulation are taken, particle is successively used 20 meshes and 50 mesh sieves, obtained Hempleaf groundsel herb granule sample A2.
Embodiment 3
1kg hempleaf groundsel herb rhizome is taken, 6 hours dry at 65 DEG C, being crushed to granularity is 40 mesh, adds 10 times of inventory of ethyl alcohol Aqueous solution (concentration is 45 weight %), ultrasonic extraction 2 times under the ultrasonic frequency of 125kHz are extracted 60 minutes, every time with 200 Purpose stainless steel wire net filtration, filtrate decompression are concentrated to the concentrate that relative density is 1.1.In concentrate be added 80g starch, The mixture (three's weight ratio is 1:0.25:1) of lactose and dextrin mixes, and is freeze-dried, collects dried cream powder, crushed 80 Mesh sets mixing channel mixing.Hempleaf groundsel herb paste, sieving granulation are taken, particle successively uses 20 meshes and 50 mesh sieves, obtains hempleaf groundsel herb Granule sample A3.
Embodiment 4
1kg hempleaf groundsel herb rhizome is taken, 10 hours dry at 50 DEG C, being crushed to granularity is 100 mesh, adds 15 times of inventory of second Alcohol solution (concentration is 40 weight %), ultrasonic extraction 2 times under the ultrasonic frequency of 125kHz are extracted 60 minutes every time, are used The stainless steel wire net filtration of 200 mesh, filtrate decompression are concentrated to the concentrate that relative density is 1.18.80g is added in concentrate The mixture (three's weight ratio is 1:0.15:1.5) of starch, lactose and dextrin mixes, and is freeze-dried, collects dried cream powder, It crushed 80 meshes, set mixing channel mixing.Hempleaf groundsel herb paste, sieving granulation are taken, particle successively uses 20 meshes and 50 mesh sieves, Obtain hempleaf groundsel herb granule sample A4.
Embodiment 5
1kg hempleaf groundsel herb rhizome is taken, 8 hours dry at 55 DEG C, being crushed to granularity is 100 mesh, adds 15 times of inventory of second Alcohol solution (concentration is 55 weight %), ultrasonic extraction 3 times under the ultrasonic frequency of 50kHz are extracted 30 minutes every time, are used The stainless steel wire net filtration of 200 mesh, filtrate decompression are concentrated to the concentrate that relative density is 1.2.50g is added in concentrate to form sediment The mixture (three's weight ratio is 1:0.25:1) of powder, lactose and dextrin mixes, and is freeze-dried, collects dried cream powder, crushes 80 meshes are crossed, mixing channel mixing is set.Hempleaf groundsel herb paste, sieving granulation are taken, particle is successively used 20 meshes and 50 mesh sieves, must be returned Soul grass granule sample A5.
Embodiment 6
1kg hempleaf groundsel herb rhizome is taken, 10 hours dry at 50 DEG C, being crushed to granularity is 50 mesh, adds 13 times of inventory of second Alcohol solution (concentration is 60 weight %), ultrasonic extraction 3 times under the ultrasonic frequency of 50kHz are extracted 30 minutes every time, are used The stainless steel wire net filtration of 200 mesh, filtrate decompression are concentrated to the concentrate that relative density is 1.13.50g is added in concentrate The mixture (three's weight ratio is 1:0.35:0.8) of starch, lactose and dextrin mixes, and is freeze-dried, collects dried cream powder, It crushed 80 meshes, set mixing channel mixing.Hempleaf groundsel herb paste, sieving granulation are taken, particle successively uses 20 meshes and 50 mesh sieves, Obtain hempleaf groundsel herb granule sample A6.
Comparative example 1
Hempleaf groundsel herb granule is prepared according to the method for embodiment 1, the difference is that methylene chloride, ethyl alcohol in step (1) Inventory with the mixed solution of ether is 8 times of hempleaf groundsel herb medicinal material, so that hempleaf groundsel herb granule sample D1 be made.
Comparative example 2
Hempleaf groundsel herb granule is prepared according to the method for embodiment 1, the difference is that methylene chloride, ethyl alcohol in step (1) Inventory with the mixed solution of ether is 20 times of hempleaf groundsel herb medicinal material, so that hempleaf groundsel herb granule sample D2 be made.
Comparative example 3
Hempleaf groundsel herb granule is prepared according to the method for embodiment 1, the difference is that using methylene chloride generation in step (1) For the mixed solution of methylene chloride, ethyl alcohol and ether, so that hempleaf groundsel herb granule sample D3 be made.
Comparative example 4
Hempleaf groundsel herb granule is prepared according to the method for embodiment 1, the difference is that replacing two with ether in step (1) The mixed solution of chloromethanes, second alcohol and water, so that hempleaf groundsel herb granule sample D4 be made.
Comparative example 5
Hempleaf groundsel herb granule is prepared according to the method for embodiment 1, the difference is that using ethanol water in step (1) Instead of methylene chloride, the mixed solution of second alcohol and water, so that hempleaf groundsel herb granule sample D5 be made.
Comparative example 6
Hempleaf groundsel herb granule is prepared according to the method for embodiment 1, the difference is that the particle in step (3) after granulation Without 20 meshes and 50 mesh sieves, so that hempleaf groundsel herb granule sample D6 be made.
Test case
(1) isoquercitrin in the hempleaf groundsel herb granule sample prepared to above-described embodiment and comparative example, hempleaf groundsel herb glucoside, Hempleaf groundsel herb polyoses content is detected, and detects the chromatographic column used as C18 chromatographic column.
(2) partial size of the hyperici,herba granule sample of above-described embodiment and comparative example preparation is detected using particles distribution instrument Distribution situation, and analytical calculation partial size is the granule number percentage U of the partial size within the scope of 0.25-0.35mm0.25-0.35
Testing result is as shown in table 1 below.
Table 1
By the result of table 1 can be seen that using method of the present invention preparation hempleaf groundsel herb granule have compared with High active component content, and particle size uniformity.
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.In skill of the invention In art conception range, can with various simple variants of the technical solution of the present invention are made, including each technical characteristic with it is any its Its suitable method is combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, is belonged to Protection scope of the present invention.

Claims (7)

1. a kind of preparation method of hempleaf groundsel herb granule, which comprises the following steps:
(1) hempleaf groundsel herb rhizome is dried, is crushed, obtain the particle that granularity is 40-100 mesh;
(2) particulate matter that step (1) obtains is mixed with ethanol water, wherein by volume, the inventory of ethanol water It is 10-15 times of the particulate matter inventory;
(3) ultrasonic extraction 2-3 times;
(4) it filters, gained filtrate decompression is concentrated to the concentrate that relative density is 1.1-1.2;
(5) concentrate that step (4) obtains is mixed with pharmaceutically acceptable auxiliary material, is freeze-dried, collect dried cream powder, It crushed 80 meshes, be placed in mixing channel mixing, obtain hempleaf groundsel herb paste;
(6) the hempleaf groundsel herb paste for obtaining step (5) is pelletized, and particle successively uses 20 meshes and 50 mesh sieves, obtains hempleaf groundsel herb Granule.
2. the method according to claim 1, wherein the concentration of the ethanol water is 40-60 weight %.
3. the method according to claim 1, wherein in step (3), the ultrasound that is used during ultrasonic extraction Wave frequency rate is 50-125kHz, and each extraction time is 30-60 minutes.
4. the method according to claim 1, wherein the auxiliary material is soluble starch, starch, lactose, sucrose At least one of with dextrin.
5. according to the method described in claim 4, it is characterized in that, the auxiliary material be starch, lactose and dextrin mixture, and The weight ratio of starch, lactose and dextrin is 1:0.01-0.5:0.1-2.
6. the hempleaf groundsel herb granule of the preparation of the method as described in any one of claim 1-5.
7. hempleaf groundsel herb granule according to claim 6, which is characterized in that the specification of the hempleaf groundsel herb granule is Every 1-3 grams is equivalent to 6-18 grams of hempleaf groundsel herb medicinal material.
CN201811508564.0A 2018-12-11 2018-12-11 A kind of hempleaf groundsel herb granule and preparation method thereof Withdrawn CN109528795A (en)

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CN117625834A (en) * 2024-01-04 2024-03-01 中国农业科学院特产研究所 SNP molecular marker based on senecio scandens ITS2 sequence and application thereof
CN117625834B (en) * 2024-01-04 2024-04-16 中国农业科学院特产研究所 SNP molecular marker based on senecio scandens ITS2 sequence and application thereof

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