CN109966449A - A kind of preparation method of Chinese materia medica preparation that treating dizziness and its preparation of preparation - Google Patents

A kind of preparation method of Chinese materia medica preparation that treating dizziness and its preparation of preparation Download PDF

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CN109966449A
CN109966449A CN201910317583.3A CN201910317583A CN109966449A CN 109966449 A CN109966449 A CN 109966449A CN 201910317583 A CN201910317583 A CN 201910317583A CN 109966449 A CN109966449 A CN 109966449A
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rhizoma
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时海燕
徐男
周丽
王鹏
李明臣
时银萍
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Shandong Qianfoshan Hospital
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Abstract

The invention belongs to traditional Chinese medicine research development fields, and in particular to a kind of preparation method of the Chinese materia medica preparation for treating dizziness and its preparation of preparation.The Chinese materia medica preparation is by dried pinellia, Rhizoma Gastrodiae, raw Rhizoma Atractylodis Macrocephalae, Poria cocos, dried orange peel, pueraria lobata, Radix Curcumae, Semen Coicis, Rhizoma Chuanxiong, 10 taste Chinese medicinal composition of Radix Glycyrrhizae；The preparation method and quality control method of said preparation are provided simultaneously, under the premise of guaranteeing that medicinal active ingredient sufficiently extracts, establish the high efficiency extraction for being suitable for mass production, refining methd, purifying purification party's active principle, reject toxic component, the Chinese medicine in-stomach floating type sustained-release preparation for clearly treating dizziness relatively with independent intellectual property right, effective substance and the mechanism of action is had developed, the multi objective quantitative finger print atlas of foundation guarantees that stable product quality is controllable.

Description

A kind of preparation method of Chinese materia medica preparation that treating dizziness and its preparation of preparation
Technical field
The invention belongs to traditional Chinese medicine research development fields, and in particular to a kind of preparation method for the Chinese materia medica preparation for treating dizziness And its preparation of preparation.
Background technique
Dizziness is Neurology, hals,Nasen und Ohrenheilkunde, internal clinic and emergency treatment common disease, frequently-occurring disease, and the cause of disease is various, machine System is complicated, is often related to multidisciplinary, multisystem lesion.Traditional Chinese medicine thinks: the main clinical manifestation of dizziness is dizzy, dim eyesight, the cause of disease In love will is unsuccessful, physically weak prolonged illness, diet internal injury, blood loss overstrain and wound, operation etc., and basic pathogenesis is wind, fire, phlegm, disturbs in the stasis of blood Empty or asthenia of essence and blood, YANG-orifices failing to be nourished, mainly with liver,spleen,kidney 3 is dirty substantial connection.This disease sees Huangdi's Internal Classics earliest. " Ling Shu Miraculous Pivot or Divine Axis sea opinion " is said: " brain being the marrow sea." say again: " marrow sea deficiency, then vertigo and tinnitus." think one disease of dizziness based on void.The Chinese Then emphasize that phlegm retention is the key factor of dizziness morbidity for Zhang Zhongjing.Later age doctor proposes that " calm do not make dizzy ", " no phlegm is not made It is dizzy ", " dizziness must be due to deficiency " etc. advocate that Zhang Shi thinks: dizziness and wind, phlegm, the stasis of blood, void are closely related, and You Yifeng, abundant expectoration are shown in.
Under modern allegro living environment, dizziness has become a kind of liability disease, and existing kind is far away in the market Needs are able to satisfy, especially have no that treat dizziness be the listing formulation application of primary symptom in clinic.The application prescription is that clinic is tested Side, also known as " dizziness side ", are treatment " wind phlegm " classic prescriptions banxia baizhu tianma decoction (" Medicine Comprehended " Qing Cheng state Peng writes) On the basis of plus pueraria lobata, Radix Curcumae, Semen Coicis, Rhizoma Chuanxiong and obtain, make full side relieve dizziness, high fever, infantile convulsions, epilepsy, etc., resolving sputum on the basis of, increase promoting the circulation of qi bowl spares, promoting blood circulationization The stasis of blood, dispelling cold and removing dampness effect, are more advantageous to treatment dizziness, and clinical efficacy is definite.Traditional Chinese medicine decoction generally can be made into granule, But preparation process is backward, clinical efficacy is not significant, and the especially not high problem of safety increasingly attracts people's attention." dizziness The monarch drug in a prescription tuber of pinellia is toxic flavour of a drug for side ", if dealing with improperly, Yi Yinqi adverse reaction.
Summary of the invention
It is also easy to produce adverse reaction for clinical proved recipe " dizziness side ", dosage is big, and administration number of times is more, and quality is unstable between batch The problems such as determining, the present invention provides a kind of preparation methods for treating dizziness Chinese materia medica preparation and multi objective quantitative finger print atlas to establish Method.
A kind of preparation method for treating dizziness Chinese materia medica preparation, comprises the steps of:
(1) Chinese medicine dried pinellia, Rhizoma Gastrodiae, raw Rhizoma Atractylodis Macrocephalae, Poria cocos, dried orange peel, pueraria lobata, Radix Curcumae, the heart of a lotus seed extraction and purification process: are measured by prescription Rice, Rhizoma Chuanxiong, Radix Glycyrrhizae crush respectively, and water mentions, and merge decoction liquor, and organic film, inorganic ceramic membrane successively filter, filtrate decompression concentration It to the clear cream of relative density 1.20~1.25, is freeze-dried, crushes, obtain medicinal extract；
(2) granule preparing process: medicinal extract and hydroxypropyl methyl cellulose in step (1) are weighed, Carbomer974, octadecyl alcolol, is gathered Ethylene adjoins pyrrolidone and mixes by equal increments method, and appropriate wetting agent is added to prepare softwood, and be sieved wet granular processed, dry；It screens out thin Whole grain is sieved in secondary granulation after powder；Gained particle can directly pack or tabletting, filling capsule use.
The recipe quantity of the step (1) are as follows: 5~20 parts of dried pinellia；10~30 parts of Rhizoma Gastrodiae；Raw 15~60 parts of Rhizoma Atractylodis Macrocephalae；Poria cocos 15~60 parts；5~20 parts of dried orange peel；10~60 parts of pueraria lobata；10~30 parts of Radix Curcumae；0~60 part of Semen Coicis；0~30 part of Rhizoma Chuanxiong；Radix Glycyrrhizae 5 ~20 parts.
Preferably, the recipe quantity of the step (1) are as follows: 10 parts of dried pinellia；15 parts of Rhizoma Gastrodiae；Raw 30 parts of Rhizoma Atractylodis Macrocephalae；30 parts of Poria cocos； 10 parts of dried orange peel；30 parts of pueraria lobata；15 parts of Radix Curcumae；30 parts of Semen Coicis；15 parts of Rhizoma Chuanxiong；10 parts of Radix Glycyrrhizae.
Organic membrane aperture of the step (1) is 500,350,200nm；The pore size of inorganic ceramic membrane of the step (1) is 100、50nm。
The condition of the filtering of the step (1) is 50-60 DEG C of temperature, pressure difference 0.10-0.15MPa；In the step (2) Medicinal extract and hydroxypropyl methyl cellulose, Carbomer974, octadecyl alcolol, polyethylene adjoin the addition mass ratio of pyrrolidone are as follows: 20:40: 15:5:4.
It is a kind of that Chinese materia medica preparation is prepared using the above method.
The method of quality control of above-mentioned Chinese materia medica preparation, comprising the following steps:
(1) HPLC finger-print is established, trigonelline, Gastrodin, liquiritin, aurantiin, aurantiamarin, different is pointed out and measure simultaneously The content of liquiritin, 8 kinds of atractylodes lactone III, enoxolone ingredients；
Chromatographic condition and system suitability InertSustain C18 chromatographic column (4.6mm × 250mm, 5 μm)；Mobile phase: Acetonitrile (A)-water (B)；Linear gradient elution time-program(me) is as follows: the min(A of 0 min → 48 %:3% → 45%)；48min→60 Min(A %:45% → 100%)；Flow velocity: 1.0mLmin-1；Detection wavelength: 254nm；Reference wavelength: 400nm；Column temperature: 30 DEG C； Sample volume: 10 μ L；Theoretical cam curve is calculated by aurantiin peak should be not less than 3000；
The preparation of reference substance solution takes trigonelline, Gastrodin, liquiritin, aurantiin, aurantiamarin, isoliquiritin, atractylodes lactone III, enoxolone reference substance is appropriate, accurately weighed, add methanol to dissolve to get；
The preparation of test solution takes the particle in step (2) appropriate, accurately weighed, finely ground, sets in stuffed conical flask, accurate Methanol 30ml is added, weighed weight is ultrasonically treated 30min, lets cool, and weighed weight is supplied the weight of loss with methanol, shaken up, Filtration, subsequent filtrate as test solution to get；
Measuring method is accurate respectively to draw reference substance solution and each 10 μ l of test solution, injects liquid chromatograph, measurement to get；
(2) quality controls: every gram of (C containing trigonelline7H7NO2), 0.10mg must not be less than；Every gram of (C containing Gastrodin13H18O3), 2.19mg must not be less than；Every gram of (C containing liquiritin21H22O9), 0.12mg must not be less than；Every gram of (C containing aurantiin27H32O14), it must not Less than 7.31mg；Every gram of (C containing aurantiamarin28H34O15), 0.13mg must not be less than；Every gram of (C containing isoliquiritin21H22O9), it must not lack In 0.17mg；Every gram of III (C containing atractylodes lactone15H20O3), 0.23mg must not be less than；Every gram of (C containing enoxolone30H46O4) meter, no It obtains and is less than 0.02mg.
The application delays on the basis of traditional decoction technique in conjunction with Modern preparations technique ultrafiltration exquisite technology, modern take orally Controlled-release technology dispels the macromoleculars toxicant such as pinellin, and exquisite active component reduces dose, increases curative effect, reduces poison Side effect；The sterile region extended in small intestine upper section absorbs, and solves the problems, such as that the daily times for spraying of compound Chinese medicinal preparation is more.To Not only Chinese medicine compound prescription Chinese medicine Integral Characteristic had been remained, but also has increased technology content, has been the complete of traditional clinical proved recipe and modern science and technology Beauty combines.
Detailed description of the invention
Fig. 1 is mixing reference substance (A), negative control solution (B) and test solution (S1, C) HPLC figure；Wherein 1, Rhizoma Gastrodiae Element；2, liquiritin；3, aurantiin；4, aurantiamarin；5, isoliquiritin；6, atractylodes lactone III；7, enoxolone
Fig. 2 is 18 batches of dizziness side's particle finger-prints.
The utility model has the advantages that
1, the Integrated Films of " ceramic membrane+organic film " refine active principle:
Contain a large amount of such as phenolic acid, flavones and saponin(e chemical component in dizziness side, wherein the Gastrodin etc. in Rhizoma Gastrodiae, in dried orange peel Aurantiamarin, aurantiin, neohesperidin etc., the researchs such as liquiritin, isoliquiritin in Radix Glycyrrhizae are more thorough, are main pharmacodynamics objects Matter.But the monarch drug in a prescription tuber of pinellia is toxicity flavour of a drug, and research finds that the macromolecular substances such as pinellin and needle-like calcium oxalate crystal are its toxic components.
The application guarantee medicinal active ingredient sufficiently extract under the premise of, establish be suitable for mass production " ceramic membrane+ The Integrated Films effectively refining method of organic film ", is conducive to:
1. dispelling the toxic components such as pinellin, reduction adverse reaction is possible, guarantees clinical application safety.
2. drastically reducing dosage, solid content removal rate reaches 75.31%, and eliminates macromolecular complex confrontation The interference of novel form auxiliary material, the perfect combination for Chinese medicine compound prescription and modern long-acting oral new agent technology provide possibility；
3. reducing subsequent treatment process, reagent and energy consumption can be greatly decreased in the produce load being especially freeze-dried, and reduced Discharge amount saves production cost, is more advantageous to industrialized production.
4. the rate of transform and filtration efficiency improve.It is first biggish organic super using aperture due to taking progressive mode Filter membrane removes the impurity such as high molecular weight protein or peptides, nucleic acid, pigment in clear liquid, not only avoids and blocks up to small aperture ceramic film Plug, efficiency improves, and the rate of transform also increases substantially.
5. film cost is changed in reduction, equipment operating cost is greatly lowered.The not raw bacterium of ceramic membrane, free from extraneous odour are reusable The advantages that, but ceramic membrane higher cost, large aperture organic film initial filter is first used, the loss of ceramic membrane can be reduced.
2, intragastric floating sustained-release preparation is modern long-acting oral preparation:
Long-acting oral preparation is not configured to extend pharmaceutical release time to 12h-24h or more, but makes drug in stomach or small intestine Upper section stay long enough, until drug all discharges within the predetermined time.
The intragastric floating sustained-release particle of the application is with hydroxypropyl methyl cellulose (HPMC) and Carbomer974 hydrophilic gel As the polymer matrices of high-crosslinking-degree, octadecyl alcolol (OA) is used as bleach activator, and PVP adjusts drug release rate as pore-foaming agent. Pass through the horizontal L of 4 factor 39(34) orthogonal preferably has studied the best preparation process of intragastric floating sustained-release particle.Test hair Existing, preferred intragastric floating sustained-release particle shows good slow release and apparent floatability, and the drug release behavior of the particle Stablize, drug effect can be maintained up to 12h or more, is able to extend release time of the drug in stomach, improves bioavilability, overcome more For number traditional Chinese medicine compounds because absorbing in small intestine upper section, and there are gastric transit time is short, gastric emptying digit rate is uncertain and influences The unfavorable physiologic factor such as drug effect.
3, core forms flavour of a drug in the comprehensive Quality Control prescription of HPLC quantitative finger print atlas:
" Chinese Pharmacopoeia " 2015 version one records the herbal species of 28 characteristic spectrums and 9 finger-prints altogether, passes through fingerprint Map has become the Feasible Mode that Chinese medicine true and false quality evaluation, quality conformance evaluation and product stability are investigated, and is general at present All over the scientific and reasonable method of quality control used.
The application establishes dizziness side's finger-print using HPLC method, and to wherein trigonelline, Gastrodin, liquiritin, shaddock 8 kinds of skin glycosides, aurantiamarin, isoliquiritin, atractylodes lactone III, enoxolone main indicator ingredients are quantitative determined, the above ingredient Recipe core group is contained into the representative ingredient of flavour of a drug, is capable of the quality of comprehensive system reflection finished dosage form, guarantees clinical treat Effect.
Specific embodiment
Pass through the preparation method and multi objective of embodiment the present invention is further explained the treatment dizziness Chinese materia medica preparation Quantitative finger print atlas method for building up, but the present invention is not limited to the contents that the following example includes.
Embodiment 1
A kind of preparation method for treating dizziness Chinese materia medica preparation, comprises the steps of:
(1) Chinese medicine dried pinellia, Rhizoma Gastrodiae, raw Rhizoma Atractylodis Macrocephalae, Poria cocos, dried orange peel, pueraria lobata, Radix Curcumae, the heart of a lotus seed extraction and purification process: are measured by prescription Rice, Rhizoma Chuanxiong, Radix Glycyrrhizae crush respectively, weigh the coarse powder between 10~20 mesh in proportion, extract 2 times, amount of water is followed successively by 10 times, 8 Times, extraction time is followed successively by 30min, 30min, merges decoction liquor, choose the organic film that aperture is 500,350,200nm, 100, The inorganic ceramic membrane of 50nm, successively filters, and 50-60 DEG C of filtration temperature, pressure difference 0.10-0.15MPa, filtrate decompression is concentrated into relatively 1.20~1.25(60 DEG C of density) clear cream, be freeze-dried, crush, obtain medicinal extract；
The recipe quantity are as follows: 10 parts of dried pinellia, 15 parts of Rhizoma Gastrodiae, raw 30 parts of Rhizoma Atractylodis Macrocephalae, 30 parts of Poria cocos, 10 parts of dried orange peel, 30 parts of pueraria lobata, 15 parts of Radix Curcumae, 30 parts of Semen Coicis, 15 parts of Rhizoma Chuanxiong；10 parts of Radix Glycyrrhizae.
(2) medicinal extract in step (1) and hydroxypropyl methyl cellulose, Carbomer974,18 granule preparing process: are weighed Alcohol, polyethylene adjoin pyrrolidone and mix (formula: medicinal extract 20mg by equal increments method；Hydroxypropyl methyl cellulose 40mg；Carbomer 15mg；Octadecyl alcolol 5mg；Polyethylene adjoins pyrrolidone 4mg), add appropriate wetting agent to prepare softwood, crosses 20 mesh Shai Zhi wet granulars, wet Grain is in 50 DEG C of dryings.40 meshes remove secondary granulation after fine powder, 20 mesh sieves.
Gained particle is directly packed.
Embodiment 2
A kind of preparation method of Chinese materia medica preparation that treating dizziness, step such as embodiment 1, only modifies recipe quantity are as follows: dried pinellia 5 Part, 10 parts of Rhizoma Gastrodiae, raw 60 parts of Rhizoma Atractylodis Macrocephalae, 60 parts of Poria cocos, 20 parts of dried orange peel, 60 parts of pueraria lobata, 10 parts of Radix Curcumae, 60 parts of Semen Coicis, 5 parts of Radix Glycyrrhizae.
Gained particle preparation is at tablet.
Embodiment 3
A kind of preparation method of Chinese materia medica preparation that treating dizziness, comprising the following steps:
(1) Chinese medicine dried pinellia, Rhizoma Gastrodiae, raw Rhizoma Atractylodis Macrocephalae, Poria cocos, dried orange peel, pueraria lobata, Radix Curcumae, the heart of a lotus seed extraction and purification process: are measured by prescription Rice, Rhizoma Chuanxiong, Radix Glycyrrhizae crush respectively, weigh the coarse powder between 10~20 mesh in proportion, extract 2 times, amount of water is followed successively by 10 times, 8 Times, extraction time is followed successively by 30min, 30min, merges decoction liquor, choose the organic film that aperture is 500,350,200nm, 100, The inorganic ceramic membrane of 50nm, successively filters, and 50-60 DEG C of filtration temperature, pressure difference 0.10-0.15MPa, filtrate decompression is concentrated into relatively 1.20~1.25(60 DEG C of density) clear cream, be freeze-dried, crush, obtain medicinal extract；
The recipe quantity are as follows: 20 parts of dried pinellia, 30 parts of Rhizoma Gastrodiae, raw 15 parts of Rhizoma Atractylodis Macrocephalae, 15 parts of Poria cocos, 5 parts of dried orange peel, 10 parts of pueraria lobata, 30 parts of Radix Curcumae, 30 parts of Rhizoma Chuanxiong；20 parts of Radix Glycyrrhizae.
(2) medicinal extract in step (1) and hydroxypropyl methyl cellulose, Carbomer974,18 granule preparing process: are weighed Alcohol, polyethylene adjoin pyrrolidone and mix (formula: medicinal extract 20mg by equal increments method；Hydroxypropyl methyl cellulose 40mg；Carbomer 15mg；Octadecyl alcolol 5mg；Polyethylene adjoins pyrrolidone 4mg), add appropriate wetting agent to prepare softwood, crosses 20 mesh Shai Zhi wet granulars, wet Grain is in 50 DEG C of dryings.40 meshes remove secondary granulation after fine powder, 20 mesh sieves.
(3) preparation of capsule: taking particle in step (2), add appropriate amount of starch, mix, it is encapsulated, be made 1000 to get.
Embodiment 4
A kind of preparation method of Chinese materia medica preparation that treating dizziness, comprising the following steps:
(1) Chinese medicine dried pinellia, Rhizoma Gastrodiae, raw Rhizoma Atractylodis Macrocephalae, Poria cocos, dried orange peel, pueraria lobata, Radix Curcumae, the heart of a lotus seed extraction and purification process: are measured by prescription Rice, Rhizoma Chuanxiong, Radix Glycyrrhizae crush respectively, weigh the coarse powder between 10~20 mesh in proportion, extract 2 times, amount of water is followed successively by 10 times, 8 Times, extraction time is followed successively by 30min, 30min, merges decoction liquor, choose the organic film that aperture is 500,350,200nm, 100, The inorganic ceramic membrane of 50nm, successively filters, and 50-60 DEG C of filtration temperature, pressure difference 0.10-0.15MPa, filtrate decompression is concentrated into relatively 1.20~1.25(60 DEG C of density) clear cream, be freeze-dried, crush, obtain medicinal extract；
The recipe quantity are as follows: 15 parts of dried pinellia, 10 parts of Rhizoma Gastrodiae, raw 60 parts of Rhizoma Atractylodis Macrocephalae, 50 parts of Poria cocos, 10 parts of dried orange peel, 50 parts of pueraria lobata, 25 parts of Radix Curcumae, 60 parts of Semen Coicis, 20 parts of Rhizoma Chuanxiong；10 parts of Radix Glycyrrhizae.
(2) medicinal extract in step (1) and hydroxypropyl methyl cellulose, Carbomer974,18 granule preparing process: are weighed Alcohol, polyethylene adjoin pyrrolidone and mix (formula: medicinal extract 20mg by equal increments method；Hydroxypropyl methyl cellulose 40mg；Carbomer 15mg；Octadecyl alcolol 5mg；Polyethylene adjoins pyrrolidone 4mg), add appropriate wetting agent to prepare softwood, crosses 20 mesh Shai Zhi wet granulars, wet Grain is in 50 DEG C of dryings.40 meshes remove secondary granulation after fine powder, 20 mesh sieves.
(3) preparation of tablet: taking particle in step (2), and 3% sodium carboxymethyl starch and 0.5% magnesium stearate is added, and mixes, Tabletting, be made 1000 to get.
Embodiment 5
The method of quality control of the Chinese materia medica preparation of embodiment 2-4, comprising the following steps:
(1) HPLC finger-print is established, trigonelline, Gastrodin, liquiritin, aurantiin, aurantiamarin, different is pointed out and measure simultaneously The content of liquiritin, 8 kinds of atractylodes lactone III, enoxolone ingredients.
Chromatographic condition and system suitability InertSustain C18 chromatographic column (4.6mm × 250mm, 5 μm)；Stream Dynamic phase: acetonitrile (A)-water (B)；Linear gradient elution time-program(me) is as follows: the min(A of 0 min → 48 %:3% → 45%)；48min → 60 min(A %:45% → 100%)；Flow velocity: 1.0mLmin-1；Detection wavelength: 254nm；Reference wavelength: 400nm；Column temperature: 30℃；Sample volume: 10 μ L.Theoretical cam curve is calculated by aurantiin peak should be not less than 3000.
The preparation of reference substance solution takes trigonelline, Gastrodin, liquiritin, aurantiin, aurantiamarin, isoliquiritin, Rhizoma Atractylodis Macrocephalae Lactone III, enoxolone reference substance are appropriate, accurately weighed, add methanol to dissolve to get.
The preparation of test solution takes the particle in step (2) appropriate, accurately weighed, finely ground, sets in stuffed conical flask, Methanol 30ml is added in precision, and weighed weight is ultrasonically treated 30min, lets cool, weighed weight is supplied the weight of loss with methanol, shaken It is even, filtration, subsequent filtrate as test solution to get.
Measuring method difference is accurate to draw reference substance solution and each 10 μ L of test solution, injects liquid chromatograph, measures, i.e., ?.
(2) every gram of this product (C containing trigonelline7H7NO2), 0.10mg must not be less than；Every gram of (C containing Gastrodin13H18O3), no It obtains and is less than 2.19mg；Every gram of (C containing liquiritin21H22O9), 0.12mg must not be less than；Every gram of (C containing aurantiin27H32O14), it must not lack In 7.31mg；Every gram of (C containing aurantiamarin28H34O15), 0.13mg must not be less than；Every gram of (C containing isoliquiritin21H22O9), it must not be less than 0.17mg；Every gram of III (C containing atractylodes lactone15H20O3), 0.23mg must not be less than；Every gram of (C containing enoxolone30H46O4) meter, it must not Less than 0.02mg.
18 batches of samples are prepared by dizziness side's intragastric floating sustained-release preparation method of granules, measure trigonelline, Gastrodin, Radix Glycyrrhizae The content of glycosides, aurantiin, aurantiamarin, isoliquiritin, atractylodes lactone III, enoxolone, the results are shown in Table 1.
8 kinds of composition measurement results (n=3) in 1 18 batches of samples of table
Comparative example 1
Extraction and purification process:
The recipe quantity are as follows: 10 parts of dried pinellia, 15 parts of Rhizoma Gastrodiae, raw 30 parts of Rhizoma Atractylodis Macrocephalae, 30 parts of Poria cocos, 10 parts of dried orange peel, 30 parts of pueraria lobata, 15 parts of Radix Curcumae, 30 parts of Semen Coicis, 15 parts of Rhizoma Chuanxiong；10 parts of Radix Glycyrrhizae.
Chinese medicine dried pinellia, Rhizoma Gastrodiae, raw Rhizoma Atractylodis Macrocephalae, Poria cocos, dried orange peel, pueraria lobata, Radix Curcumae, Semen Coicis, Rhizoma Chuanxiong, Radix Glycyrrhizae point are measured by prescription It does not crush, weighs the coarse powder between 10~20 mesh in proportion, extract 2 times, amount of water is followed successively by 10 times, 8 times, and extraction time is successively For 30min, 30min, merge decoction liquor, it is spare after sampling.
Filtrate after hyperfiltration process weighing is equally divided into 4 points, and 1 part is 1. original liquid, in addition passes through 2. aperture respectively for 3 parts For the organic film of 500,350,200nm, 100, the inorganic ceramic membrane of 50nm；3. the 100, inorganic ceramic membrane of 50nm；4. aperture is 500, the organic film of 350,200nm, using HPLC method measurement trigonelline, Gastrodin, liquiritin, aurantiin, aurantiamarin, different sweet The content of careless glycosides, atractylodes lactone III, enoxolone, and sample solid content is measured, it the results are shown in Table 2.
2 distinct methods upgrading result of table compares (%)
Note: solid content removal rate (%)=(stoste total solid-ultrafiltrate total solid)/stoste total solid × 100%；The rate of transform (%)=penetrating fluid component content/original liquid component total amount × 100%；Mean transferred rate (%)=(trigonelline+Rhizoma Gastrodiae Element+liquiritin+aurantiin+aurantiamarin+isoliquiritin+III+enoxolone of atractylodes lactone)/8 × 100%
Comparative example 2
Granule preparing process:
The recipe quantity are as follows: 10 parts of dried pinellia, 15 parts of Rhizoma Gastrodiae, raw 30 parts of Rhizoma Atractylodis Macrocephalae, 30 parts of Poria cocos, 10 parts of dried orange peel, 30 parts of pueraria lobata, 15 parts of Radix Curcumae, 30 parts of Semen Coicis, 15 parts of Rhizoma Chuanxiong；10 parts of Radix Glycyrrhizae.
Chinese medicine dried pinellia, Rhizoma Gastrodiae, raw Rhizoma Atractylodis Macrocephalae, Poria cocos, dried orange peel, pueraria lobata, Radix Curcumae, Semen Coicis, Rhizoma Chuanxiong, Radix Glycyrrhizae point are measured by prescription It does not crush, weighs the coarse powder between 10~20 mesh in proportion, extract 2 times, amount of water is followed successively by 10 times, 8 times, and extraction time is successively For 30min, 30min, merge decoction liquor, chooses the organic film that aperture is 500,350,200nm, 100, the inorganic ceramic of 50nm Film successively filters, and 50-60 DEG C of filtration temperature, pressure difference 0.10-0.15MPa, filtrate decompression is concentrated into relative density 1.20~1.25 The clear cream of (60 DEG C) is freeze-dried, and is crushed, is obtained medicinal extract；
Orthogonal is the best preparation process for determining dizziness side's intragastric floating sustained-release particle, is investigated in single factor experiment On the basis of, prescription medicinal extract dosage is 20mg, with hydroxypropyl methyl cellulose (HPMC), carbomer (Carbomer) 974,18 It is investigation factor that alcohol (OA), polyethylene, which adjoin pyrrolidone (PVP) dosage, using drift time and accumulative releasing degree as inspection target, according to According to L9(34) orthogonal test scheme tested, preparation process is carried out preferably, to determine optimal parameter.Factor level is shown in Table 3.With Release requires and floating particle comprehensive score is as evaluation index, preferably optimal preparation prescription.
High spot reviews particle rise drift time and 2 time points Cumulative release amount: the floating particle 2h release the drug 30%, In 12h drug release 90%, drift time 3s is played, with the cumulative release percentage Q2 and Q12 and drift time T in 2h and 12h of making pellet And the sum of ideal value deviation Y be inspection target, i.e. Y=| Q2-30% | × 100+ | Q12-90% | × 100+ | T-3 |.It the results are shown in Table 4, Variance analysis is shown in Table 5.
Flotation property takes by intragastric floating sustained-release particle obtained by orthogonal test table, 37 DEG C of steady temperature is placed in, in perseverance Determining revolving speed is 75rmin-1, the 0.1molL of 900mL-1In hydrochloric acid solution, its floatability is observed under the conditions of simulation peristole Can, it takes float slow release particle to be placed in and turns in basket, rotation basket, which has been put into, has observed drift time and lasting flotation time.
Release in vitro Performance precision is weighed by intragastric floating sustained-release particle in dizziness side's obtained by orthogonal test table 100mg carries out Accumulation dissolution measurement by the first law regulation in Chinese Pharmacopoeia two annex drug release determination methods of version in 2015.It will Sample is placed in the simulation simulated gastric fluid of 500mL pH1.5, and control revolving speed is 100rmin-1, temperature is 37.0 ± 0.5 DEG C, according to Method measurement, in 1,2,4,8,12,18, for 24 hours, fixed point is accurate respectively measures release solution 1mL, and supplements mutually synthermal, phase simultaneously The blank dissolution medium 1mL of same volume discards primary filtrate with 0.45 μm of filtering with microporous membrane, and precision measures 5 μ L of subsequent filtrate, note Enter high performance liquid chromatograph, measure peak area of the Gastrodin at 245nm wavelength, and substitutes into calibration curve equation calculating accumulation and release Degree of putting draws release profiles according to measurement result.Drug accumulation release=[Rt/L] × 100.Wherein, Rt indicates medicine in the t time The Cumulative release amount of object, L indicate the drug total amount being initially loaded into.
Variance analysis is according to standards of grading Y, as shown in Table 2, the influence size order of each factor are as follows: A > B > C > D, it is optimal Group is combined into A2B1C1D1.I.e. hydroxypropyl methyl cellulose, Carbomer974, octadecyl alcolol, polyethylene adjoin pyrrolidone mass ratio: 40:15: 5:4.
Confirmatory experiment is tested according to preferred best preparation process, and parallel laboratory test 3 times.As a result 3 experiments are made dizzy Dizzy side's intragastric floating sustained-release particles float and accumulative releasing degree are preferable, consistent with orthogonal experiments.The 2h in simulated gastric fluid Average accumulated release≤30%.Particle plays drift, and dissolution rate > 80% of duration > 8h, 8h in 3s, meets in stomach The quality requirement of float slow release particle.It the results are shown in Table 6.
3 factor level table of table
4 Orthogonal experiment results of table
5 the results of analysis of variance of table
Note: F0.05 (2,2)=19.00
The release performance of 6 intragastric floating sustained-release particle of table measures (n=3)

Claims (8)

1. a kind of preparation method for treating dizziness Chinese materia medica preparation, which is characterized in that comprise the steps of:
(1) Chinese medicine dried pinellia, Rhizoma Gastrodiae, raw Rhizoma Atractylodis Macrocephalae, Poria cocos, dried orange peel, pueraria lobata, Radix Curcumae, the heart of a lotus seed extraction and purification process: are measured by prescription Rice, Rhizoma Chuanxiong, Radix Glycyrrhizae crush respectively, and water mentions, and merge decoction liquor, and organic film, inorganic ceramic membrane successively filter, filtrate decompression concentration It to the clear cream of relative density 1.20~1.25, is freeze-dried, crushes, obtain medicinal extract；
(2) medicinal extract and hydroxypropyl methyl cellulose (HPMC), carbomer in step (1) granule preparing process: are weighed (Carbomer) 974, octadecyl alcolol (OA), polyethylene adjoin pyrrolidone (PVP) and mix by equal increments method, and appropriate wetting agent is added to prepare Softwood, be sieved wet granular processed, dry；Secondary granulation after fine powder is screened out, whole grain is sieved；Coating solution coating is added, it is dry；Gained Grain can directly pack or tabletting, filling capsule use.
2. preparation method according to claim 1, which is characterized in that the recipe quantity of the step (1) are as follows: dried pinellia 5~ 20 parts；10~30 parts of Rhizoma Gastrodiae；Raw 15~60 parts of Rhizoma Atractylodis Macrocephalae；15~60 parts of Poria cocos；5~20 parts of dried orange peel；10~60 parts of pueraria lobata；Radix Curcumae 10 ~30 parts；0~60 part of Semen Coicis；0~30 part of Rhizoma Chuanxiong；5~20 parts of Radix Glycyrrhizae.
3. preparation method according to claim 1, which is characterized in that the recipe quantity of the step (1) are as follows: dried pinellia 10 Part；15 parts of Rhizoma Gastrodiae；Raw 30 parts of Rhizoma Atractylodis Macrocephalae；30 parts of Poria cocos；10 parts of dried orange peel；30 parts of pueraria lobata；15 parts of Radix Curcumae；30 parts of Semen Coicis；15 parts of Rhizoma Chuanxiong； 10 parts of Radix Glycyrrhizae.
4. preparation method according to claim 1, which is characterized in that organic membrane aperture of the step (1) be 500, 350,200nm；The pore size of inorganic ceramic membrane of the step (1) is 100,50nm.
5. preparation method according to claim 1, which is characterized in that the condition of the filtering of the step (1) is temperature 50- 60 DEG C, pressure difference 0.10-0.15MPa.
6. preparation method according to claim 1, which is characterized in that medicinal extract and hydroxypropyl methyl in the step (2) Cellulose (HPMC), carbomer (Carbomer) 974, octadecyl alcolol (OA), polyethylene adjoin the addition mass ratio of pyrrolidone (PVP) Are as follows: 12:60:10:5:6.
7. Chinese materia medica preparation is prepared using preparation method described in claim 1-6.
8. a kind of method of quality control of Chinese materia medica preparation as claimed in claim 7, which comprises the following steps:
(1) HPLC finger-print is established, trigonelline, Gastrodin, liquiritin, aurantiin, aurantiamarin, different is pointed out and measure simultaneously The content of liquiritin, 8 kinds of atractylodes lactone III, enoxolone ingredients；
Chromatographic condition and system suitability InertSustain C18 chromatographic column (4.6mm × 250mm, 5 μm)；Mobile phase: Acetonitrile (A)-water (B)；Linear gradient elution time-program(me) is as follows: the min(A of 0 min → 48 %:3% → 45%)；48min→60 Min(A %:45% → 100%)；Flow velocity: 1.0mLmin-1；Detection wavelength: 254nm；Reference wavelength: 400nm；Column temperature: 30 DEG C； Sample volume: 10 μ L；Theoretical cam curve is calculated by aurantiin peak should be not less than 3000；
The preparation of reference substance solution takes trigonelline, Gastrodin, liquiritin, aurantiin, aurantiamarin, isoliquiritin, atractylodes lactone III, enoxolone reference substance is appropriate, accurately weighed, add methanol to dissolve to get；
The preparation of test solution takes the particle in step (2) appropriate, accurately weighed, finely ground, sets in stuffed conical flask, accurate Methanol 30ml is added, weighed weight is ultrasonically treated 30min, lets cool, and weighed weight is supplied the weight of loss with methanol, shaken up, Filtration, subsequent filtrate as test solution to get；
Measuring method is accurate respectively to draw reference substance solution and each 10 μ L of test solution, injects liquid chromatograph, measurement to get；
(2) quality controls: every gram of (C containing trigonelline7H7NO2), 0.10mg must not be less than；Every gram of (C containing Gastrodin13H18O3), no It obtains and is less than 2.19mg；Every gram of (C containing liquiritin21H22O9), 0.12mg must not be less than；Every gram of (C containing aurantiin27H32O14), it must not lack In 7.31mg；Every gram of (C containing aurantiamarin28H34O15), 0.13mg must not be less than；Every gram of (C containing isoliquiritin21H22O9), it must not be less than 0.17mg；Every gram of III (C containing atractylodes lactone15H20O3), 0.23mg must not be less than；Every gram of (C containing enoxolone30H46O4) meter, it must not Less than 0.02mg.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110579539A (en) * 2019-07-11 2019-12-17 神威药业集团有限公司 Establishing method of fingerprint of Huaganjian tea
CN110806457A (en) * 2019-11-29 2020-02-18 南京南医堂健康产业发展有限公司 Detection method of fingerprint of Sijun manna drink
CN112691113A (en) * 2021-02-08 2021-04-23 山东省中医药研究院 Pharmaceutical composition for preventing and treating hypertensive inflammatory response and application thereof
CN112891466A (en) * 2021-03-15 2021-06-04 杭州师范大学 Traditional Chinese medicine composition for preventing and treating phlegm-dampness obstructing type hypertension and quality control method

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110579539A (en) * 2019-07-11 2019-12-17 神威药业集团有限公司 Establishing method of fingerprint of Huaganjian tea
CN110579539B (en) * 2019-07-11 2021-08-06 神威药业集团有限公司 Establishing method of fingerprint of Huaganjian tea
CN110806457A (en) * 2019-11-29 2020-02-18 南京南医堂健康产业发展有限公司 Detection method of fingerprint of Sijun manna drink
CN110806457B (en) * 2019-11-29 2021-10-08 南京南医堂健康产业发展有限公司 Detection method of fingerprint of Sijun manna drink
CN112691113A (en) * 2021-02-08 2021-04-23 山东省中医药研究院 Pharmaceutical composition for preventing and treating hypertensive inflammatory response and application thereof
CN112691113B (en) * 2021-02-08 2022-06-24 山东省中医药研究院 Pharmaceutical composition for preventing and treating hypertension inflammatory reaction and application thereof
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