CN108653387A - Linggui zhugan decoction compound granule and preparation method thereof - Google Patents
Linggui zhugan decoction compound granule and preparation method thereof Download PDFInfo
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- CN108653387A CN108653387A CN201810670486.8A CN201810670486A CN108653387A CN 108653387 A CN108653387 A CN 108653387A CN 201810670486 A CN201810670486 A CN 201810670486A CN 108653387 A CN108653387 A CN 108653387A
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 63
- 239000008187 granular material Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 244000037364 Cinnamomum aromaticum Species 0.000 claims abstract description 41
- 235000014489 Cinnamomum aromaticum Nutrition 0.000 claims abstract description 41
- 239000000341 volatile oil Substances 0.000 claims abstract description 41
- 239000000284 extract Substances 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 235000008599 Poria cocos Nutrition 0.000 claims abstract description 26
- 244000197580 Poria cocos Species 0.000 claims abstract description 26
- 238000000605 extraction Methods 0.000 claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 25
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- 239000001947 glycyrrhiza glabra rhizome/root Substances 0.000 claims abstract description 23
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- 235000019410 glycyrrhizin Nutrition 0.000 description 7
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- 206010007558 Cardiac failure chronic Diseases 0.000 description 3
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- 208000009525 Myocarditis Diseases 0.000 description 1
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- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
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Classifications
-
- 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
- A61K36/06—Fungi, e.g. yeasts
- A61K36/07—Basidiomycota, e.g. Cryptococcus
- A61K36/076—Poria
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/28—Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
- A61K36/284—Atractylodes
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
- A61K36/484—Glycyrrhiza (licorice)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/54—Lauraceae (Laurel family), e.g. cinnamon or sassafras
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1605—Excipients; Inactive ingredients
- A61K9/1629—Organic macromolecular compounds
- A61K9/1652—Polysaccharides, e.g. alginate, cellulose derivatives; Cyclodextrin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P9/00—Drugs for disorders of the cardiovascular system
- A61P9/04—Inotropic agents, i.e. stimulants of cardiac contraction; Drugs for heart failure
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Animal Behavior & Ethology (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Mycology (AREA)
- Biotechnology (AREA)
- Microbiology (AREA)
- Medical Informatics (AREA)
- Botany (AREA)
- Alternative & Traditional Medicine (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Cardiology (AREA)
- Hospice & Palliative Care (AREA)
- Heart & Thoracic Surgery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of linggui zhugan decoction compound granules and preparation method thereof.The preparation method specifically includes, 4 parts of raw material Poria cocos, 3 parts of cassia twig, 3 parts of Rhizoma Atractylodis Macrocephalae, 2 parts of honey-fried licorice root are weighed by weight, cassia twig, Rhizoma Atractylodis Macrocephalae are carried out to steam distillation respectively and obtain volatile oil component, 8 12 times of water progress water are added with Poria cocos and honey-fried licorice root in its residue to carry, extraction 12 hours, are extracted 13 times every time, freeze-dried powder is made in extract, and auxiliary material is added, particle is made, then the volatile oil is sprayed into particle surface obtained to get linggui zhugan decoction compound granule.It is stable quality, good in taste, easy to carry and take using granule product made from preparation method of the present invention, while the pharmaceutical activity of linggui zhugan decoction compound granule can be kept well.The present invention also provides a kind of linggui zhugan decoction compound granulars and preparation method thereof.
Description
Technical field
The invention belongs to Chinese native medicine compound prescription pellet technical fields, and in particular to a kind of Chinese medicine compound prescription linggui zhugan decoction compound granular
Agent and preparation method thereof.
Background technology
The clinical manifestation category Chinese medicine " palpitaition " of chronic heart failure, " oedema ", " phlegm and retained fluid ", " dyspnea ", " obstruction of the heart qi ", " exhaustion of vital energy at the critical stage of an illness "
Equal scopes, card belong to asthenia in origin and asthenia in superficiality, this void is mostly the deficiency of vital energy, the deficiency of yang, marks actually water, wet, phlegm, stasis of blood mutual resistance, the deficient and weak YANG QI of the heart is it
Pathology emphasis, the heart-yang deficiency of vital energy are that the morbidity of this disease is crucial, and always through chronic heart failure pathology, QI invigorating Wen Yang is its basic therapy.
Linggui zhugan decoction comes from Han dynasty Zhang Zhongjing《Treatise on Febrile and Miscellaneous Disease》, by Poria cocos, cassia twig, Rhizoma Atractylodis Macrocephalae, four taste Chinese medicine group of Radix Glycyrrhizae
At, its inverse " epigastric fullness, upward adverseness of gas to the chest, the dizziness when getting up " that cures mainly that the heart is insufficiency of the spleen-yang, drink is stopped the supple of gas or steam (《The Treatise on Fevrile Diseases distinguishes that sun abnormal pulse is demonstrate,proved
And it controls》) and " distention and fullness in the chest and hypochondrium, dizzy ", " losing heart " card (《Synopsis Golden Chamber phlegmatic cough's abnormal pulse is demonstrate,proved and is controlled》), be warm heart-yang,
Invigorating the spleen gas, the classics recipe for changing water drink.Full side selects medicine precise and appropriate, and compatibility is reasonable, and bowl spares, which has, rushes down, simultaneous treatment of principal and subordinate symptoms, eliminating evil without hindering just,
The effect of playing QI invigorating Wen Yang, sharp water altogether, hit heart failure pathogenic characteristic, and the party is widely used in treating cardiovascular disease
Each stage and various illnesss, as unstable angina pectoris, arrhythmia cordis, myocarditis, cardiovascular disease merge chronic heart function not
Entirely, chronic congestive heart failure, high blood pressure, cardiogenic shock, Cardiorenal syndrome etc., it is curative for effect.
Existing linggui zhugan decoction is mainly decoction, and inconvenience is brought to patient on.Decoction is that tcm clinical practice is most normal
Conventional dosage forms are convenient for diagnosis and treatment based on an overall analysis of the illness and the patient's condition, addition or subtraction of changes, but its poor taste, and inconvenient to carry, patient is difficult to receive.Existing skill
Art kind also has part linggui zhugan decoction to be prepared into pill or tablet, but pill, tablets and other formulations, absorbs relatively poor, slowly effect,
It is difficult to adapt to the application of acute disease, and patient is poor to the compliance of this dosage form.Chinese herbal granules are in traditional Chinese herbal decoction and dried molassed
The novel form to grow up on the basis of the dosage forms such as slurry agent had not only remained decoction and has absorbed feature fast, that effect is rapid, but also overcome
Decoction faces the used time and decocts that inconvenient, dose is big, poor taste, easily mould lose the shortcomings of rotten and pill, tablet absorption difference, takes effect
Slow deficiency is a kind of suitable formulations for treating angiocardiopathy.In addition, the preparation process of granule is suitable for industrial production,
Product quality is stablized, and takes, carries, storing, transporting more convenient, but there has been no granule agent is made in linggui zhugan decoction at present
The product of type, also without pertinent literature record or relevant report.
Invention content
In view of this, it is an object of the invention to overcome existing linggui zhugan decoction agent poor taste, inconvenient to carry, Siberian cocklebur osmanthus art
Sweet soup pill, tablets and other formulations, the problems such as absorbing relatively poor, slowly effect, provide a kind of linggui zhugan decoction compound granule and
Preparation method and a kind of preparation method of linggui zhugan decoction freeze-dried powder.
By further investigation and many experiments it has surprisingly been found that during preparing linggui zhugan decoction granule, first will
Cassia twig, Rhizoma Atractylodis Macrocephalae carry out steam distillation and obtain volatile oil component, then its residue and Poria cocos and liquorice are carried out water and carry and be made particle,
Volatile oil is finally sprayed into particle surface obtained again, the drug of linggui zhugan decoction compound granule can be kept to live well
Property, while living by the drug that a large amount of experiment discovery extracting factor can influence to be made compound granule to some extent
Property, thus creatively obtain technical scheme of the present invention.
Heretofore described granule (Granules) refers to coordinating drug and suitable auxiliary material and manufactured particle
Shape preparation;Heretofore described particle refers to Chinese medicinal granule, is made of the extracted concentration of the prepared slices of Chinese crude drugs, does not add
Any auxiliary material, particle for tcm clinical practice formula, Chinese medicinal granule are handled by following process, and particle can be made
A variety of dosage forms such as agent, coated granule, capsule.
The present invention provides a kind of preparation method of linggui zhugan decoction compound granule, includes the following steps:
Following raw materials are weighed by following weight part ratio:4 parts of Poria cocos, 3 parts of cassia twig, 3 parts of Rhizoma Atractylodis Macrocephalae, 2 parts of honey-fried licorice root;
Cassia twig and Rhizoma Atractylodis Macrocephalae are subjected to steam distillation respectively, obtain Ramulus Cinnamomi Volatile oil ingredient, Baizhu volatile oil ingredient;
Poria cocos, honey-fried licorice root is added in cassia twig and Rhizoma Atractylodis Macrocephalae residue, 8~12 times of water are added and extract, extraction time is 1~2
Hour, it extracts 1~3 time, extraction is preferably ultra-pure water with water;
Extract is carried out to be freeze-dried obtained linggui zhugan decoction freeze-dried powder;
Linggui zhugan decoction freeze-dried powder obtained is mixed and is sieved with auxiliary material, ethyl alcohol is added and is made softwood, sieving is made
It is granular, it is dried under vacuum to constant weight;Wherein, the auxiliary material can be the common auxiliary material for preparing granule, as starch, lactose, dextrin,
Icing Sugar, calcium sulfate, sucrose, mannitol, microcrystalline cellulose, glucose etc., wherein sieve used in sifting step is made after softwood
14 mesh sieve is selected as in network optimization;
The Ramulus Cinnamomi Volatile oil, Baizhu volatile oil are sprayed on particle obtained to get linggui zhugan decoction compound granule.
Further, the preparation method of the linggui zhugan decoction compound granule, wherein extracted in described plus water
In step, extraction time is preferably 3 times.
Further, the preparation method of the linggui zhugan decoction compound granule, wherein extracted in described plus water
In step, preferably every time 1.5 hours extraction time.
Further, the preparation method of the linggui zhugan decoction compound granule, wherein extracted in described plus water
In step, the multiple that water is added is preferably 8 times of water.
Further, the preparation method of the linggui zhugan decoction compound granule, wherein the auxiliary material is Icing Sugar and paste
The weight ratio of essence, linggui zhugan decoction freeze-dried powder and Icing Sugar, dextrin is 1:3:3.
Further, the preparation method of the linggui zhugan decoction compound granule, wherein the auxiliary material is soluble starch
And dextrin, linggui zhugan decoction freeze-dried powder and soluble starch, dextrin weight ratio be 1:1:1.
Further, the preparation method of the linggui zhugan decoction compound granule, wherein the second that the ethyl alcohol is 50%
Alcohol, the vacuum drying temperature are 50~60 DEG C.
Further, the preparation method of the linggui zhugan decoction compound granule, in obtained linggui zhugan decoction compound granular
Further include the steps that packing compound granule obtained after agent.
The present invention also provides a kind of linggui zhugan decoction compound granule, the linggui zhugan decoction compound granule is by above-mentioned
Obtained by one preparation method.
The present invention also provides a kind of preparation methods of linggui zhugan decoction compound granular, include the following steps:
Following raw materials are weighed by following weight part ratio:4 parts of Poria cocos, 3 parts of cassia twig, 3 parts of Rhizoma Atractylodis Macrocephalae, 2 parts of honey-fried licorice root;
Cassia twig and Rhizoma Atractylodis Macrocephalae are subjected to steam distillation respectively, obtain Ramulus Cinnamomi Volatile oil ingredient and Baizhu volatile oil ingredient;
Poria cocos, Radix Glycyrrhizae is added in cassia twig and Rhizoma Atractylodis Macrocephalae residue, 8~12 times of water are added and extract, extraction time is every time 1~
It 2 hours, extracts 1~3 time, extraction is preferably ultra-pure water with water;
Extract is carried out to be freeze-dried to obtain linggui zhugan decoction freeze-dried powder;
The Ramulus Cinnamomi Volatile oil, Baizhu volatile oil are sprayed into linggui zhugan decoction freeze-dried powder, obtain linggui zhugan decoction particle.
Further, the preparation method of the linggui zhugan decoction compound granular, wherein in the step that described plus water extracts
In rapid, extraction time is 3 times, and extraction time is 1.5 hours every time, and the multiple that water is added is 8 times of water.
The present invention also provides a kind of linggui zhugan decoction compound granular, the linggui zhugan decoction compound granular is according to any of the above-described
Obtained by the preparation method of the linggui zhugan decoction particle.
It by the linggui zhugan decoction compound granular obtained by the present invention, is handled by following process, granule, packet can be made
A variety of dosage forms such as clothing particle, capsule.
The present invention carries out quality control using UPLC (ultra performance liquid chromatography) technology, can effectively control the matter of compound granular
Amount, using linggui zhugan decoction compound granule made from technical solution of the present invention, product quality is stablized, good in taste, make without pair
With can make daily health caring, take for a long time, take, carry, storing, transporting more convenient, and ensureing its drug to the maximum extent
Activity keeps it to prevent the effect of the angiocardiopathies such as chronic heart failure.
It should be understood that foregoing general description and following detailed description are all exemplary, and it is intended to carry
For the further explanation of claimed technology.
Description of the drawings
The embodiment of the present invention is described in more detail in conjunction with the accompanying drawings, the above and other purposes of the present invention,
Feature and advantage will be apparent.Attached drawing is used for providing further understanding the embodiment of the present invention, and constitutes explanation
A part for book is not construed as limiting the invention for explaining the present invention together with the embodiment of the present invention.Except non-clearly referring to
Go out, otherwise attached drawing is not considered as drawn to scale.In the accompanying drawings, identical reference label typically represents same components or step.
In the accompanying drawings:
Fig. 1 shows UPLC (ultra performance liquid chromatography) figure of each technic index of linggui zhugan decoction particle reference substance of the present invention
Spectrum;
Fig. 2 shows each technic index UPLC (ultra high efficiencies of linggui zhugan decoction particle made from according to embodiments of the present invention 5
Liquid chromatogram) collection of illustrative plates;
Specific implementation mode
In order to enable the object, technical solutions and advantages of the present invention become apparent, root is described in detail below with reference to accompanying drawings
According to example embodiments of the present invention.Obviously, described embodiment is only a part of the embodiment of the present invention, rather than this hair
Bright whole embodiments, it should be appreciated that the present invention is not limited by example embodiment described herein.Based on reality described herein
Example is applied, those skilled in the art's obtained all other embodiment in the case where not making the creative labor should all be fallen into
Within protection scope of the present invention.In the present description and drawings, it will use the same reference numerals to represent substantially the same
Element and function, and by omission to the duplicate explanation of these elements and function.
(1) preparation method of linggui zhugan decoction compound granule:
Embodiment 1:
Linggui zhugan decoction compound granule is prepared as follows:
Weigh Poria cocos 12g, cassia twig 9g, Rhizoma Atractylodis Macrocephalae 9g and honey-fried licorice root 6g;
Cassia twig and Rhizoma Atractylodis Macrocephalae are distilled with vapor respectively, obtain Ramulus Cinnamomi Volatile oil ingredient and Baizhu volatile oil ingredient;
Poria cocos, honey-fried licorice root is added in cassia twig and Rhizoma Atractylodis Macrocephalae residue, the ultra-pure waters that 8 times of amounts are added extract, and extraction time is
It 1.5 hours every time, extracts 3 times;
Extract is carried out to be freeze-dried to obtain linggui zhugan decoction freeze-dried powder;
By linggui zhugan decoction freeze-dried powder obtained and soluble starch, dextrin according to weight ratio 1:1:1 ratio mixing is simultaneously
Softwood is made in sieving, the ethyl alcohol for being added 50%, and sieving is made graininess, is dried under vacuum to constant weight at 60 DEG C, sprays into the osmanthus
Branch, Baizhu volatile oil, obtain linggui zhugan decoction compound granule;
Gained linggui zhugan decoction compound granule can be packed, 3 bags of granules can be packaged into.
Embodiment 2:
Linggui zhugan decoction compound granule is prepared as follows:
Weigh Poria cocos 12g, cassia twig 9g, Rhizoma Atractylodis Macrocephalae 9g and honey-fried licorice root 6g;
Cassia twig and Rhizoma Atractylodis Macrocephalae are distilled with vapor respectively, obtain Ramulus Cinnamomi Volatile oil ingredient and Baizhu volatile oil ingredient;
Poria cocos, honey-fried licorice root is added in cassia twig and Rhizoma Atractylodis Macrocephalae residue, the ultra-pure waters that 8 times of amounts are added extract, and extraction time is
It 1.5 hours every time, extracts 3 times;
Extract is carried out to be freeze-dried to obtain linggui zhugan decoction freeze-dried powder;
By linggui zhugan decoction freeze-dried powder obtained and Icing Sugar, dextrin according to weight ratio 1:3:3 ratio is mixed and is sieved, and is added
Softwood is made in the ethyl alcohol for entering 50%, and sieving is made graininess, is dried under vacuum to constant weight at 50 DEG C, sprays into the cassia twig, Rhizoma Atractylodis Macrocephalae
Volatile oil obtains linggui zhugan decoction compound granule.
Embodiment 3:
Linggui zhugan decoction compound granule is prepared as follows:
Weigh Poria cocos 12g, cassia twig 9g, Rhizoma Atractylodis Macrocephalae 9g and honey-fried licorice root 6g;
Cassia twig and Rhizoma Atractylodis Macrocephalae are distilled with vapor respectively, obtain Ramulus Cinnamomi Volatile oil ingredient and Baizhu volatile oil ingredient;
Poria cocos, honey-fried licorice root is added in cassia twig and Rhizoma Atractylodis Macrocephalae residue, the ultra-pure waters that 8 times of amounts are added extract, and extraction time is
It 1 hour every time, extracts 2 times;
Extract is carried out to be freeze-dried to obtain linggui zhugan decoction freeze-dried powder;
By linggui zhugan decoction freeze-dried powder obtained and soluble starch, dextrin according to weight ratio 1:1:1 ratio mixing is simultaneously
Softwood is made in sieving, the ethyl alcohol for being added 50%, and sieving is made graininess, is dried under vacuum to constant weight at 50 DEG C, sprays into the osmanthus
Branch, Baizhu volatile oil, obtain linggui zhugan decoction compound granule.
Embodiment 4:
Linggui zhugan decoction compound granule is prepared as follows:
Weigh Poria cocos 12g, cassia twig 9g, Rhizoma Atractylodis Macrocephalae 9g and honey-fried licorice root 6g;
Cassia twig and Rhizoma Atractylodis Macrocephalae are distilled with vapor respectively, obtain Ramulus Cinnamomi Volatile oil ingredient and Baizhu volatile oil ingredient;
Poria cocos, honey-fried licorice root is added in cassia twig and Rhizoma Atractylodis Macrocephalae residue, the ultra-pure waters that 12 times of amounts are added extract, and extraction time is
It 2 hours every time, extracts 1 time;
Extract is carried out to be freeze-dried to obtain linggui zhugan decoction freeze-dried powder;
By linggui zhugan decoction freeze-dried powder obtained and soluble starch, dextrin according to weight ratio 1:1:1 ratio mixing is simultaneously
Softwood is made in sieving, the ethyl alcohol for being added 60%, and sieving is made graininess, is dried under vacuum to constant weight at 60 DEG C, sprays into the osmanthus
Branch, Baizhu volatile oil, obtain linggui zhugan decoction compound granule.
Embodiment 5:
Linggui zhugan decoction compound granular is prepared as follows:
Weigh Poria cocos 12g, cassia twig 9g, Rhizoma Atractylodis Macrocephalae 9g and honey-fried licorice root 6g;
Cassia twig and Rhizoma Atractylodis Macrocephalae are distilled with vapor respectively, obtain cassia twig, Baizhu volatile oil ingredient;
Poria cocos, honey-fried licorice root is added in cassia twig and Rhizoma Atractylodis Macrocephalae residue, the ultra-pure waters that 8 times of amounts are added extract, and extraction time is
It 1.5 hours every time, extracts 3 times;
Extract is carried out to be freeze-dried to obtain linggui zhugan decoction freeze-dried powder;
The Ramulus Cinnamomi Volatile oil, Baizhu volatile oil are sprayed into, linggui zhugan decoction compound granular is obtained.
Embodiment 6:
Linggui zhugan decoction compound granular is prepared as follows:
Weigh Poria cocos 12g, cassia twig 9g, Rhizoma Atractylodis Macrocephalae 9g and honey-fried licorice root 6g;
Cassia twig and Rhizoma Atractylodis Macrocephalae are distilled with vapor respectively, obtain cassia twig, Baizhu volatile oil ingredient;
Poria cocos, honey-fried licorice root is added in cassia twig and Rhizoma Atractylodis Macrocephalae residue, the ultra-pure waters that 12 times of amounts are added extract, and extraction time is
It 2 hours every time, extracts 1 time;
Extract is carried out to be freeze-dried to obtain linggui zhugan decoction freeze-dried powder;
The Ramulus Cinnamomi Volatile oil, Baizhu volatile oil are sprayed into, linggui zhugan decoction compound granular is obtained.
Embodiment 7:
Linggui zhugan decoction compound granular is prepared as follows:
Weigh Poria cocos 12g, cassia twig 9g, Rhizoma Atractylodis Macrocephalae 9g and honey-fried licorice root 6g;
Cassia twig and Rhizoma Atractylodis Macrocephalae are distilled with vapor respectively, obtain cassia twig, Baizhu volatile oil ingredient;
Poria cocos, honey-fried licorice root is added in cassia twig and Rhizoma Atractylodis Macrocephalae residue, the ultra-pure waters that 12 times of amounts are added extract, and extraction time is
It 1 hour every time, extracts 2 times;
Extract is carried out to be freeze-dried to obtain linggui zhugan decoction freeze-dried powder;
The Ramulus Cinnamomi Volatile oil, Baizhu volatile oil are sprayed into, linggui zhugan decoction compound granular is obtained.
(2) the technic index assay of linggui zhugan decoction compound granular:
Using liquiritin, cinnamic acid, cinnaldehydrum, glycyrrhizic acid, atractylodes lactone III, dry extract yield as technic index, to using
The index content of linggui zhugan decoction compound granule made from the method for the present invention is measured.
Institute using sensing equipment includes:The Waters Acquity UPLC H-Class ultra performance liquid chromatography systems (U.S.
Waters companies), KQ3200DB types ultrasonic cleaning machine (Fauna of Kunshan, Jiangsu ultrasonic instrument Co., Ltd), BP211D type electronic balances
(German Sartorius companies).
Institute using measure reagent includes:Chromatographic Pure Methanol, trifluoroacetic acid aqueous solution, chromatography pure phosphoric acid.
The preparation of reference substance standard curve:
It is appropriate that precision weighs liquiritin, cinnamic acid, cinnaldehydrum, glycyrrhizic acid and III reference substance of atractylodes lactone, is respectively placed in
In the brown measuring bottle of 10mL, adds methanol to dissolve and be settled to scale, shake up, obtain reference substance storing solution;
The accurate above-mentioned reference substance storing solution of absorption is a certain amount of successively again, is placed in the brown measuring bottle of same 10mL, first is added
Alcohol is settled to scale, shakes up, and is configured to every 1mL and contains liquiritin, cinnamic acid, cinnaldehydrum, glycyrrhizic acid, atractylodes lactone III respectively
The mixed reference substance solution of 47.06,2.75,159.80,34.32,3.61 μ g is filtered through 0.45 μm of miillpore filter.
Precision draws 0.2,0.5,1,2,3,4,5,6,7,8 μ L of mixed reference substance solution, injects in liquid chromatograph, measures
The peak area of liquiritin, cinnamic acid, cinnaldehydrum, glycyrrhizic acid and atractylodes lactone III, using peak area as ordinate (Y), mixing control
The sample introduction quality of product is abscissa (X), draws standard curve, calculates regression equation.Specially:Equation of linear regression is Y=
7896X-12369, r=0.9997, the results showed that, liquiritin sample size is in good linear relationship in 9.41-376.48 μ g;Linearly
Regression equation is Y=22045X-4220, r=0.9992, the results showed that, cinnamic acid sample size is in 0.55-22.00 μ g in good
Linear relationship;Equation of linear regression is Y=1699X-14184, r=0.9997, the results showed that, cinnaldehydrum sample size is in 31.96-
1278.40 μ g are in good linear relationship;Equation of linear regression is Y=1787X-961, r=0.9998, the results showed that, glycyrrhizic acid
Sample size is in good linear relationship in 6.86-274.56 μ g;Equation of linear regression is Y=17267X-2615, r=0.9993, knot
Fruit shows III sample size of atractylodes lactone in 0.72-28.88 μ g in good linear relationship.
Chromatographic condition:Chromatographic column is Waters Acquity UPLC BEH C18 columns (100mm × 2.1mm, 1.7 μm);Stream
Dynamic is mutually -0.05% phosphate aqueous solution of acetonitrile, gradient elution:0-8min, 5%-32% acetonitrile;8-17min, 32%-95% second
Nitrile;17-20min, 95%-5% acetonitrile;Volume flow 0.2mL/min;30 DEG C of column temperature;Detection wavelength 227nm.
It is test article to take the sweet particle of Siberian cocklebur osmanthus art that 5 method of above-described embodiment is prepared, and passes through above-mentioned ultra high efficiency liquid phase color
Spectrum is analyzed.The analysis collection of illustrative plates of reference substance as shown in Figure 1, wherein retention time be 7.822 minutes, 11.520 minutes,
Peak at 12.185 minutes, 12.645 minutes, 14.619 minutes is respectively:1 it is liquiritin, 2 be cinnamic acid, 3 is cinnaldehydrum, 4
It is the corresponding peaks atractylodes lactone III for glycyrrhizic acid, 5.The analysis collection of illustrative plates of test article is as shown in Fig. 2, corresponding reference substance analyzes collection of illustrative plates
The retention time of each technic index at 7.810 minutes 1 is the corresponding peak of liquiritin in figure, at 11.514 minutes 2 is cinnamic acid pair
The peak answered, at 12.180 minutes 3 be the corresponding peak of cinnaldehydrum, at 12.645 minutes 4 be the corresponding peak of glycyrrhizic acid, 14.614 minutes
Place 5 is the corresponding peaks atractylodes lactone III.3 analysis verifications are carried out to test article, obtain liquiritin, cinnamic acid, cinnaldehydrum, sweet
Oxalic acid, atractylodes lactone III, extract extracted amount average content be respectively 1.09mg/g, 0.32mg/g, 6.58mg/g,
1.35mg/g, 0.0059mg/g, 257.24mg/g, and relative error is respectively less than 5%.It is visible through the invention by test data
The sweet compound granular product of Siberian cocklebur osmanthus art and the sweet compound granule product of Siberian cocklebur osmanthus art that extraction process obtains can retain preferable drug
Activity, and product quality is stablized.
(3) property of linggui zhugan decoction compound granule measures:
Angle of repose measures:
The linggui zhugan decoction compound granule product being prepared in 1 method of embodiment carries out angle of repose survey as test article
It is fixed, obtain granule product angle of repose θ<30℃.Angular data of stopping shows the good fluidity of the granule, reaches medical particle
Agent product requirement.Either method known to a person skilled in the art can be used in the assay method at angle of repose, and such as injection method excludes
Method, gradient method etc. are measured.
Melting inspection:
The linggui zhugan decoction compound granule product being prepared in 1 method of embodiment takes 9 grams of granules as test article,
9 grams of granules are equivalent to the amount for the granule for being packaged into one bag, heat water 200mL, stir 5 minutes, observe immediately, solvable
Particle all dissolves.
It should be noted that purpose of the term as used in this specification merely for description particular implementation, rather than
It is intended to limit the invention.Unless the context clearly indicates otherwise, otherwise singulative as used herein
" one ", "one" and "the" are also intended to including plural form.The terms "include", "comprise" or its any other variant are intended to contain
Lid non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also include other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.In the absence of more restrictions, the element limited by sentence " including ... ", it is not excluded that including
There is also other identical elements in the process, method, article or equipment of the element.
Those skilled in the art should understand that be:The above embodiments are only used to illustrate the technical solution of the present invention., and
It is non-that it is limited;Although present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art can
With technical scheme described in the above embodiments is modified, either which part or all technical features are carried out etc.
With replacement;And these modifications or replacements, the range of it does not separate the essence of the corresponding technical solution claims of the present invention.
Claims (10)
1. a kind of preparation method of linggui zhugan decoction compound granule, includes the following steps:
Following raw materials are weighed by following weight part ratio:4 parts of Poria cocos, 3 parts of cassia twig, 3 parts of Rhizoma Atractylodis Macrocephalae, 2 parts of honey-fried licorice root;
Cassia twig and Rhizoma Atractylodis Macrocephalae are subjected to steam distillation respectively, obtain Ramulus Cinnamomi Volatile oil ingredient and Baizhu volatile oil ingredient;
Poria cocos, honey-fried licorice root is added in cassia twig and Rhizoma Atractylodis Macrocephalae residue, 8~12 times of water are added and extract, extraction time is 1~2 hour,
Extraction 1~3 time;
Extract is carried out to be freeze-dried obtained linggui zhugan decoction freeze-dried powder;
Linggui zhugan decoction freeze-dried powder obtained is mixed and is sieved with auxiliary material, ethyl alcohol is added, softwood is made, graininess is made in sieving,
It is dried under vacuum to constant weight;
The Ramulus Cinnamomi Volatile oil, Baizhu volatile oil are sprayed into get linggui zhugan decoction compound granule.
2. preparation method according to claim 1, wherein in the step of described plus water extracts, times of water is added
Number is 8 times of water, and extraction time is 3 times, and extraction time is 1.5 hours every time.
3. preparation method according to claim 1, wherein the auxiliary material is Icing Sugar and dextrin, linggui zhugan decoction freeze-dried powder
Weight ratio with Icing Sugar, dextrin is 1:3:3.
4. preparation method according to claim 1, wherein the auxiliary material is soluble starch and dextrin, linggui zhugan decoction
The weight ratio of freeze-dried powder and soluble starch, dextrin is 1:1:1.
5. preparation method according to claim 1, wherein the ethyl alcohol that the ethyl alcohol is 50%, the vacuum drying temperature
It is 50~60 DEG C.
6. also being wrapped after obtained linggui zhugan decoction compound granule according to any preparation method in Claims 1 to 5
Include the step of being packed compound granule obtained.
7. a kind of linggui zhugan decoction compound granule is made according to any preparation method in claim 1~6.
8. a kind of preparation method of linggui zhugan decoction compound granular, includes the following steps:
Following raw materials are weighed by following weight part ratio:4 parts of Poria cocos, 3 parts of cassia twig, 3 parts of Rhizoma Atractylodis Macrocephalae, 2 parts of honey-fried licorice root;
Cassia twig and Rhizoma Atractylodis Macrocephalae are subjected to steam distillation respectively, obtain Ramulus Cinnamomi Volatile oil ingredient and Baizhu volatile oil ingredient;
Poria cocos, honey-fried licorice root is added in cassia twig and Rhizoma Atractylodis Macrocephalae residue, 8~12 times of water are added and extract, extraction time is 1~2 hour,
Extraction 1~3 time;
Extract is carried out to be freeze-dried to obtain linggui zhugan decoction freeze-dried powder;
The Ramulus Cinnamomi Volatile oil, Baizhu volatile oil are sprayed into linggui zhugan decoction freeze-dried powder, obtain linggui zhugan decoction particle.
9. the preparation method of linggui zhugan decoction compound granular according to claim 8, wherein extracted in described plus water
The step of in, the multiple that water is added is 8 times of water, and extraction time is 3 times, and extraction time is every time 1.5 hours.
10. a kind of linggui zhugan decoction compound granular is made according to any preparation method in claim 8 or 9.
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