CN110559379A - Preparation method of pure traditional Chinese medicine powder decoction granules - Google Patents

Preparation method of pure traditional Chinese medicine powder decoction granules Download PDF

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Publication number
CN110559379A
CN110559379A CN201910922013.7A CN201910922013A CN110559379A CN 110559379 A CN110559379 A CN 110559379A CN 201910922013 A CN201910922013 A CN 201910922013A CN 110559379 A CN110559379 A CN 110559379A
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decoction
traditional chinese
chinese medicine
granule
weight
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高小康
董阳
胡姣
付真真
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Hubei Shennong Hanfang Biotechnology Co Ltd
Hubei University of Medicine
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Hubei Shennong Hanfang Biotechnology Co Ltd
Hubei University of Medicine
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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)
    • A61K36/23Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
    • A61K36/232Angelica
    • 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)
    • A61K36/23Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
    • A61K36/233Bupleurum
    • AHUMAN NECESSITIES
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    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/23Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
    • A61K36/236Ligusticum (licorice-root)
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    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/31Brassicaceae or Cruciferae (Mustard family), e.g. broccoli, cabbage or kohlrabi
    • 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)
    • A61K36/48Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
    • A61K36/484Glycyrrhiza (licorice)
    • 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)
    • A61K36/65Paeoniaceae (Peony family), e.g. Chinese peony
    • 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)
    • A61K36/71Ranunculaceae (Buttercup family), e.g. larkspur, hepatica, hydrastis, columbine or goldenseal
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/73Rosaceae (Rose family), e.g. strawberry, chokeberry, blackberry, pear or firethorn
    • A61K36/736Prunus, e.g. plum, cherry, peach, apricot or almond
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/88Liliopsida (monocotyledons)
    • A61K36/89Cyperaceae (Sedge family)
    • A61K36/8905Cyperus (flatsedge)
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    • 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
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P25/00Drugs for disorders of the nervous system
    • A61P25/06Antimigraine agents
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • 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
    • A61K2236/331Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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    • A61K2236/39Complex extraction schemes, e.g. fractionation or repeated extraction steps
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    • 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

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Abstract

A method for preparing Chinese medicinal granule. The preparation method comprises five steps, namely a first decoction process, a second solid-liquid separation technology, a third concentration process, a fourth drying process and a fifth granulation process. The invention is used for pure Chinese medicinal powder decoction granules.

Description

preparation method of pure traditional Chinese medicine powder decoction granules
Technical Field
The invention relates to a preparation method of pure traditional Chinese medicine powder decoction granules.
Background
migraine is a common clinical neurovascular disease, has high morbidity, is manifested by periodic attack and difficult recovery, and seriously affects the physical health and the life quality of the majority of patients. At present, most scholars think that migraine is mainly caused by cerebrovascular contraction and relaxation dysfunction and the imbalance of ratio of serum endothelin (E7w) Calcitonin Gene Related Peptide (CGRP), western medicines have single action mechanism, no effective method for treating migraine and no comprehensive regulation on the clinical treatment of migraine, so that a unique clinical syndrome differentiation treatment system of the traditional Chinese medicine is paid more and more attention. Modern medical research shows that the ligusticum wallichii contains volatile oil, ferulic acid and ligustrazine; radix Paeoniae alba contains various organic acids volatile oil and penoniflorin, and has effects of improving cerebral circulation, tranquilizing mind and relieving pain.
The ancient famous prescription powder soup is prepared from two volumes of dialectical records of Qing dynasty famous doctors and old soldiers, and contains eight traditional Chinese medicinal materials of ligusticum wallichii, liquorice, angelica dahurica, white paeony root, bunge cherry seed, radix bupleuri, rhizoma cyperi and semen brassicae. According to the actual clinical application and scientific research of hundreds of years, the decoction has obvious curative effect on treating the migraine. At present, few researches on migraine treatment by using disperse decoction are conducted on the whole world, and most of the researches are directly taking decoction. For a long time, although the traditional Chinese medicine decoction mode is gradually refined and perfected in the aspects of human medicine form, decoction apparatus, method and the like, the traditional Chinese medicine decoction mode has the defects of individual operation of families, extensive decoction process, lack of quantitative indexes, inconvenience in carrying and taking and the like.
Disclosure of Invention
The invention aims to provide a preparation method of pure traditional Chinese medicine granular powder decoction, which optimizes and standardizes the production and preparation process of the granular powder decoction and fully extracts effective substances.
the above purpose is realized by the following technical scheme:
A process for preparing the Chinese-medicinal particles 'powdered decoction' includes such steps as decocting, solid-liquid separation, concentrating, drying and granulating.
The preparation method of the pure traditional Chinese medicine decoction granules comprises the first step of decoction process, 41.3g of ligusticum wallichii, 20.65g of radix paeoniae alba, 12.39g of semen brassicae, 8.26g of rhizoma cyperi, 4.13g of bunge cherry seed, 4.13g of liquorice, 4.13g of radix bupleuri and 0.03g of radix angelicae are weighed, 8 times of water is added, the mixture is boiled for 30min each time for 2 times, the decoction is filtered, the decoction is combined, and the mixture is frozen and dried after being concentrated under reduced pressure.
The preparation method of the pure traditional Chinese medicine decoction granule comprises the step two of solid-liquid separation technology, and the decoction and the granule of the decoction are prepared by a hot high-speed centrifugation method.
the preparation method of the pure traditional Chinese medicine decoction granules comprises a third step of concentration process, wherein the two decoctions obtained in the second step are concentrated to 40 ~ 60mL by a rotary evaporator at the temperature of 50 ~ 70 ℃.
the preparation method of the pure traditional Chinese medicine decoction of partial decoction is characterized in that in the fourth step of drying process, decoction of partial decoction of the pure traditional Chinese medicine is dried in a spray drying mode or a drying mode of normal pressure drying or vacuum drying, the drying temperature is 50 ~ 70 ℃, the obtained particles are hollow spherical particles, and the density is 200 ~ 600kg/m3
The preparation method of the pure traditional Chinese medicine powder decoction granules comprises the fifth step of granulation process, wherein the powder decoction traditional Chinese medicine granules are granulated by a wet method or a dry method.
The pure traditional Chinese medicine powder decoction granules comprise 40-42g of ligusticum wallichii, 20-21g of white paeony root, 12-13g of semen brassicae, 8-9g of rhizoma cyperi, 4-5g of bunge cherry seed, 4-5g of liquorice, 4-5g of radix bupleuri and 0.02-0.04g of radix angelicae.
The pure traditional Chinese medicine decoction granule is prepared from 41.3g of ligusticum wallichii, 20.65g of radix paeoniae alba, 12.39g of semen brassicae, 8.26g of rhizoma cyperi, 4.13g of bunge cherry seed, 4.13g of liquorice, 4.13g of radix bupleuri and 0.03g of radix angelicae.
The pure traditional Chinese medicine decoction granules are prepared from 40g of ligusticum wallichii, 20g of radix paeoniae alba, 12g of semen brassicae, 8g of rhizoma cyperi, 4g of bunge cherry seed, 4g of liquorice, 4g of radix bupleuri and 0.02g of radix angelicae.
The pure traditional Chinese medicine decoction granules are prepared from 42g of ligusticum wallichii, 21g of radix paeoniae alba, 13g of semen brassicae, 9g of rhizoma cyperi, 5g of bunge cherry seed, 5g of liquorice, 5g of radix bupleuri and 0.04g of radix angelicae.
Has the advantages that:
1. Compared with wet granulation, the dry granulation of the invention can shorten the process route, reduce the dosage of auxiliary materials, and the prepared granules have better appearance shape and dissolubility, are particularly suitable for special traditional Chinese medicine materials with humidity sensitivity, extremely easy solubility, sugar content and the like, are also the main process in the granulation production of traditional Chinese medicine formula granules, can improve the production efficiency, reduce the labor cost and reduce the single dose.
The ligusticum wallichii adopted by the invention has the effects of promoting blood circulation and promoting qi circulation, dispelling wind and relieving pain, and can disperse and go up to the top of the mountain; enter the blood system and descend to reach the blood sea; promoting blood circulation and removing blood stasis, and is suitable for various diseases caused by blood stasis; has good effects of dispelling pathogenic wind and relieving pain, and can be used for treating headache due to wind evil and wind-damp arthralgia; has effects in dispelling pungent components, relieving depression, dredging meridians, and relieving pain.
the white peony root adopted by the invention has the functions of calming the liver, relieving pain, nourishing blood, regulating menstruation, astringing yin, arresting sweating and enriching blood.
The white mustard seed adopted by the invention has the effects of benefiting qi and eliminating phlegm, warming spleen and stomach for dispelling cold, dredging collaterals and relieving pain, warming lung and eliminating phlegm and benefiting qi, and eliminating mammary gland stagnation and dredging collaterals and relieving pain; can be used for treating cough and asthma due to cold phlegm, distending pain in chest and hypochondrium, phlegm stagnation in channels and collaterals, numbness and pain of joints, phlegm dampness and fluid injection, and carbuncle of yin and swelling.
The rhizoma cyperi adopted by the invention has the effects of dispersing stagnation of liver qi, soothing liver-qi stagnation, promoting qi circulation to relieve pain, relieving liver depression and qi stagnation, distending pain in chest and hypochondrium, hernia pain and epigastric pain caused by cold congealing and qi stagnation. It also has effects in dispersing stagnated liver qi, regulating menstruation and relieving pain, and can be used for treating menoxenia, amenorrhea, dysmenorrhea and breast pain; it also enters spleen meridian, and has the effects of relieving epigastric distention, promoting digestion and descending qi.
The bunge cherry seeds adopted by the invention have the effects of moistening lung, smoothing intestine, descending qi and inducing diuresis, and can treat symptoms such as large intestine qi stagnation, dryness, unsmooth urination, dysuria, large abdominal edema, edema of limbs, beriberi and the like.
The liquorice adopted by the invention has the functions of tonifying spleen, tonifying qi, moistening lung, relieving cough, relieving spasm and pain, and moderating and harmonizing traditional Chinese medicines, and the liquorice can also moderate the side effect of severe medicines, harmonize the medicines, and the raw liquorice also has the functions of clearing heat and removing toxicity.
the radix bupleuri adopted by the invention has the effects of harmonizing exterior and interior, soothing liver-qi stagnation, lifting yang and sinking, abating fever and preventing malaria, and can be used for treating cold and fever, alternating chills and fever, malaria, liver depression and qi stagnation, chest and rib distending pain, rectocele, uterine prolapse and irregular menstruation.
The angelica dahurica adopted by the invention has the functions of expelling wind-damp, promoting blood circulation, expelling pus, promoting granulation and relieving pain; can be used for treating headache, toothache, nasosinusitis, hemorrhoid, leucorrhea with red and white discharge, carbuncle, cellulitis, pyocutaneous disease, and skin pruritus.
The specific implementation mode is as follows:
Example 1:
A process for preparing the Chinese-medicinal particles 'powdered decoction' includes such steps as decocting, solid-liquid separation, concentrating, drying and granulating.
Example 2:
The preparation method of the pure traditional Chinese medicine decoction granules in embodiment 1 comprises the first step of decoction, weighing 41.3g of ligusticum wallichii, 20.65g of radix paeoniae alba, 12.39g of semen brassicae, 8.26g of rhizoma cyperi, 4.13g of semen pruni, 4.13g of liquorice, 4.13g of radix bupleuri and 0.03g of radix angelicae, adding 8 times of water, boiling for 30min each time for 2 times, filtering, combining decoction liquids, concentrating under reduced pressure, and freeze-drying. The raw materials of the standard decoction of the bulk drugs are derived from Chinese medicinal decoction pieces of eight medicinal materials in genuine producing areas or main producing areas, and the decoction is standardized according to the clinical decoction method according to the Chinese medicinal theory.
Example 3:
In the method for preparing the pure traditional Chinese medicine decoction granule in example 1, the solid-liquid separation technology in the second step is to prepare the decoction and the granule of the decoction by a hot high-speed centrifugation method.
In the traditional decoction, a hot filtering method is usually adopted, and the filter material is generally non-woven fabric. With the technological progress, the high-speed centrifugation and membrane separation technology with the characteristics of high efficiency, energy conservation, greenness and the like replaces the traditional filtration method.
Example 4:
the preparation method of the pure traditional Chinese medicine decoction granule in embodiment 1 comprises a third step of concentration, wherein the two decoctions in the second step are concentrated to 40 ~ 60mL by a rotary evaporator at a temperature of 50 ~ 70 ℃.
The equipment and method in the traditional Chinese medicine concentration process of the decoction of traditional Chinese medicine and the concentration ratio of the extracting solution are important research control points. The vacuum concentration method is widely used in production because it is suitable for concentrating a liquid medicine containing a heat-sensitive component, and has the characteristics of high evaporation efficiency and short concentration time.
Example 5:
the preparation method of the pure traditional Chinese medicine decoction pieces of powdered traditional Chinese medicine is described in embodiment 1, the fourth step is a drying process, the decoction pieces of the powdered traditional Chinese medicine decoction pieces are dried by spray drying or normal pressure drying or vacuum drying, the drying temperature is 50 ~ 70 ℃, the obtained particles are hollow spherical particles, the density is 200 ~ 600kg/m3, and good dissolubility, dispersibility, fluidity and the like are obtained.
Example 6:
in the fifth granulating process of the preparation method of pure traditional Chinese medicine decoction granule of example 1, the decoction traditional Chinese medicine granule is granulated by a wet method or a dry method.
Example 7:
The pure traditional Chinese medicine powder decoction granules comprise 40-42g of ligusticum wallichii, 20-21g of white paeony root, 12-13g of semen brassicae, 8-9g of rhizoma cyperi, 4-5g of bunge cherry seed, 4-5g of liquorice, 4-5g of radix bupleuri and 0.02-0.04g of radix angelicae.
Example 8:
the pure traditional Chinese medicine decoction granule of embodiment 7, the ligusticum wallichii is 41.3g, the radix paeoniae alba is 20.65g, the semen brassicae is 12.39g, the rhizoma cyperi is 8.26g, the bunge cherry seed is 4.13g, the liquorice is 4.13g, the radix bupleuri is 4.13g, and the radix angelicae is 0.03 g.
Example 9:
The pure traditional Chinese medicine decoction granule of embodiment 7, the ligusticum wallichii, the radix paeoniae alba, the semen brassicae, the rhizoma cyperi, the bunge cherry seed, the liquorice, the radix bupleuri and the radix angelicae dahuricae are 40g, 12g, 8g, 4g and 4g, respectively.
example 10:
The pure traditional Chinese medicine decoction granule of embodiment 7, the ligusticum wallichii, the radix paeoniae alba, the semen brassicae, the rhizoma cyperi, the bunge cherry seed, the liquorice, the radix bupleuri and the radix angelicae are respectively 42g, 13g, 9g, 5g and 0.04 g.
Example 11:
The preparation method of the pure traditional Chinese medicine decoction granule comprises the steps of exploring an extraction process of effective substances of the decoction, determining proper extraction solvent, decoction times, water addition amount and decoction time, and fully extracting the effective substances by taking a decoction formula as a starting material; establishing a high performance liquid chromatography fingerprint spectrum or a characteristic spectrum; on the basis of extracting effective substances, researching proper operation methods and conditions of concentration, granulation and drying, and determining proper auxiliary materials and proportion of medicines and auxiliary materials; optimizes and standardizes the production and preparation process of the traditional Chinese medicine granule of the dispersible decoction.

Claims (10)

1. A preparation method of pure traditional Chinese medicine decoction granules is characterized by comprising five steps of a first decoction process, a second solid-liquid separation technology, a third concentration process, a fourth drying process and a fifth granulation process.
2. The preparation method of the pure traditional Chinese medicine decoction granules according to claim 1, wherein in the first decoction process, 41.3g of ligusticum wallichii, 20.65g of radix paeoniae alba, 12.39g of semen brassicae, 8.26g of rhizoma cyperi, 4.13g of semen pruni, 4.13g of liquorice, 4.13g of radix bupleuri and 0.03g of radix angelicae are weighed, 8 times of water is added, each time of boiling is 30min for 2 times, filtering is carried out, decoction solutions are combined, and after the pressure reduction and concentration, the decoction solutions are freeze-dried.
3. the method for preparing pure Chinese medicinal granule of dispersible decoction according to claim 1, wherein the second solid-liquid separation technique comprises hot high-speed centrifugation to obtain decoction and granule.
4. the preparation method of the pure traditional Chinese medicine decoction granule as claimed in claim 1, wherein the concentration process of the third step is to concentrate the two decoctions of the second step to 40 ~ 60mL by a rotary evaporator at 50 ~ 70 ℃.
5. the method for preparing pure Chinese medicinal granule of dispersible decoction according to claim 1, wherein the fourth drying step comprises spray drying, drying under normal pressure or vacuum drying at 50 ~ 70 deg.C to obtain hollow spherical granule with density of 200 ~ 600kg/m3
6. the method for preparing the pure traditional Chinese medicine granule for treating the migraine according to claim 1, wherein in the fifth granulation process, the traditional Chinese medicine granule for treating the migraine is prepared by wet granulation or dry granulation.
7. The pure traditional Chinese medicine powder decoction granules comprise 40-42g of ligusticum wallichii, 20-21g of white paeony root, 12-13g of semen brassicae, 8-9g of rhizoma cyperi, 4-5g of bunge cherry seed, 4-5g of liquorice, 4-5g of radix bupleuri and 0.02-0.04g of radix angelicae.
8. The pure traditional Chinese medicine decoction granule as claimed in claim 7, which is characterized in that the ligusticum wallichii is 41.3g by weight, the radix paeoniae alba is 20.65g by weight, the semen brassicae is 12.39g by weight, the rhizoma cyperi is 8.26g by weight, the bunge cherry seed is 4.13g by weight, the liquorice is 4.13g by weight, the radix bupleuri is 4.13g by weight, and the radix angelicae is 0.03g by weight.
9. the pure traditional Chinese medicine decoction granule as claimed in claim 7, wherein the weight parts of the ligusticum wallichii is 40g, the white peony root is 20g, the white mustard seed is 12g, the nutgrass galingale rhizome is 8g, the bunge cherry seed is 4g, the licorice root is 4g, the radix bupleuri is 4g, and the radix angelicae is 0.02 g.
10. the pure traditional Chinese medicine decoction granule as claimed in claim 7, wherein the rhizoma Chuanxiong is 42g, the radix paeoniae alba is 21g, the semen brassicae is 13g, the rhizoma cyperi is 9g, the semen pruni is 5g, the radix glycyrrhizae is 5g, the radix bupleuri is 5g, and the radix angelicae is 0.04 g.
CN201910922013.7A 2019-09-27 2019-09-27 Preparation method of pure traditional Chinese medicine powder decoction granules Pending CN110559379A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116019870A (en) * 2023-03-14 2023-04-28 济南市中医医院 Application of traditional Chinese medicine composition in preparation of medicine for treating headache

Citations (5)

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Publication number Priority date Publication date Assignee Title
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