CN102940708A - Traditional Chinese medicine chewable tablet for treating upper respiratory tract infection and preparation method of chewable tablet - Google Patents
Traditional Chinese medicine chewable tablet for treating upper respiratory tract infection and preparation method of chewable tablet Download PDFInfo
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Abstract
The invention discloses a traditional Chinese medicine chewable tablet for treating upper respiratory tract infection and a preparation method of the chewable tablet. The traditional Chinese medicine chewable tablet is a solid preparation prepared from radix scutellariae extractive, jasmine extractive and medical additives according to proper proportions and proper procedures; and the traditional Chinese medicine chewable tablet can not only effectively resist against virus and sterilize, but also has such functions as clearing heat, anti-inflammatory and analgesia, etc. Compared with the common tablets, the traditional Chinese medicine chewable tablet disclosed by the invention has the advantages of good taste, quick absorption, fast effect taking, strong action, good compliance and the like, is convenient to take, and is especially suitable for elders, children and swallowing difficulty patients. The invention further discloses a quality detecting method of the traditional Chinese medicine chewable tablet. The quality detecting method comprises verifying, checking and content measuring procedures. The precision of the quality control method is high, the reproducibility is good, the recovery is high, the preparation quality can be effectively guaranteed, and the clinic treatment effect is fully guaranteed.
Description
Technical field
The present invention relates to a kind of Chewable Tablets of Chinese traditional medicine and preparation and quality determining method for the treatment of upper respiratory tract infection, belong to technical field of Chinese medicines.
Background technology
Upper respiratory tract infection is the general name of nose, pharynx, laryngitis, be commonly called as " flu ", " cold ", a kind of commonly encountered diseases, frequently-occurring disease, life, study and work impact on people are very big, and main manifestations is the symptoms such as heating, headache, throat pain, cough, nasal obstruction watery nasal discharge, sneeze, systemic pain and antiadoncus.
Modern medicine thinks that this disease is caused by antibacterial or viral infection, and wherein virus and the infection that jointly causes of antibacterial account for 90%, such as untimely processing, may merge or the multiple severe infections of secondary, even threaten the mankind's (especially child and old man) life.Doctor trained in Western medicine is take symptomatic treatment as main, and independent antibacterial infects uses antibiotic, and independent viral infection there is no active drug with medicines such as acyclovir, amantadine hydrochloride, ribavirins to antibacterial and the viral infection that jointly causes.
Motherland's medical science thinks that primary disease belongs to the calentura category, the treatment rule of main employing the " heat is then trembled with fear it ".This case history history of Chinese traditional treatment is long, accumulated abundant clinical experience, modern times have also been found multiple Chinese medicine and the compound recipe thereof that has antiviral, antibacterial action and improve patient part and General Symptoms, and a series of Chinese patent medicines have in succession been developed, relate to the dosage forms such as tablet, granule, pill, oral liquid, capsule, injection, freeze-dried powder, such as Radix Isatidis granules, YINQIAO JIEDU PIAN, SHUANGHUANGLIAN KOUFUYE with connect and spend clearly pestilence capsule etc.
At present, the toxic and side effects of chemical synthetic drug is by extensive cognition, the existence of Resistant strain in some patients were allergy or the body so that antibiotic utilization limited to, the desirable antiviral drugs of curative effect cans be counted on one's fingers, clinically in the urgent need to having definite antibiotic and antiviral dual function and medicine rapid-action, drug safety.Chinese medicine comes from natural, and exogenous pollution and toxic and side effects are all humbleer, has no drug resistance, and has outstanding advantage in treatment aspect virus and bacterial infectious disease.Therefore, adopt modern pharmaceutical technology and biological assessment ways and means, one or more effective ingredient in Chinese extracts are carried out organic assembling make the modern Chinese medicine preparation, both having can be clinician and patient provides more medication to select, and can have a tremendous social and economic benefits again.
The former side of medicine of the present invention comes from Yuan Dynasty's Luo Tianyi " precious mirror of hygiene rolls up 17 " Huangqin Qingfei Decoction, and former dosage form is decoction.But the side's of considering taste of Chinese medicine Radix Scutellariae, Fructus Gardeniae all have bitterness, and baicalin is less stable in aqueous solution, therefore the present invention is made into solid dosage forms, by adding suitable adjuvant, cover the bitterness of medicine, to remedy the deficiency of decoction, oral liquid.
Chewable tablet has not only that conventional tablet is easy to carry, stable in properties, the simple characteristics of preparation technology, also has following advantage: need not disintegrating procedue, and good dispersing state, drug-eluting speed is fast, absorbs rapidly; Can directly act on respiratory tract, greatly improve bioavailability, curative effect is better; Taking convenience need not with mixing in water for oral taking or takes; Absorb by oral mucosa after chewing, mouthfeel is good, can reduce the gastrointestinal untoward reaction, and compliance is good, especially is fit to old man, child and the patient of difficulty that swallows.Simultaneously, the technology that chewable tablet is prepared into the Sugarless type preparation is comparatively ripe, can enlarge the sufferer crowd and be particularly useful for vast diabetics and take.For antibacterial or the viral upper respiratory tract infection that causes, the used medicine of its treatment requires must be rapid-action, and effect is rapid, so the present invention selects chewable tablet as the research and development dosage form, be beneficial to take, and can reach the effect of quick acting, satisfy better the needs of patient's medication.
Summary of the invention
For above deficiency of the prior art, the purpose of this invention is to provide a kind of Chewable Tablets of Chinese traditional medicine for the treatment of upper respiratory tract infection.This Chewable Tablets of Chinese traditional medicine belongs to compound Chinese medicinal preparation, can take stopgap measures, antiviral, antibiotic effectively has the effects such as analgesic, antiinflammatory, analgesia simultaneously, can also reach and use the requirement safe, quality controllable, that bioavailability is high, taking dose is little, easy to carry, rapid-action.
A further object of the present invention provides the preparation method of the Chewable Tablets of Chinese traditional medicine of above-mentioned treatment upper respiratory tract infection.
An also purpose of the present invention provides the quality determining method of the Chewable Tablets of Chinese traditional medicine of above-mentioned treatment upper respiratory tract infection.
The present invention is based on motherland's medical science to understanding and the Therapeutic Principle of upper respiratory tract infection, with reference to clinical application experience and modern pharmacology achievement in research, filter out the Chinese medicine that has heat-clearing and toxic substances removing, lets out fiery relieving restlessness effect, by the theory of Chinese medical science prescription, adopt modern pharmacy technological achievement the other side Chinese medicine to extract purification, make the modern Chinese medicine preparation, set up quality determining method.
Chewable Tablets of Chinese traditional medicine of the present invention is with crude drug and the pharmaceutic adjuvant of suitable percentage by weight, makes according to certain technological process.Wherein, crude drug refers to Radix Scutellariae extract and these two kinds of active component of Fructus Gardeniae extract.Radix Scutellariae extract comes from baikal skullcap root, and the nature and flavor bitter cold has heat clearing and damp drying, lets out the effect of fire detoxifcation, the excess-heat of kind lung heat clearing fire and the part of the body cavity above the diaphragm housing the heart and lungs, and baicalin is the main effective ingredient of Radix Scutellariae extract.Fructus Gardeniae extract comes from the Chinese medicine Fructus Gardeniae, and the nature and flavor bitter cold has heat clearing away, pathogenic fire purging, and the effect of removing heat from blood can be let out clearly the fire of three warmers, the relieving restlessness that clears away heart-fire, jasminoidin is the main effective ingredient of Fructus Gardeniae extract.Pharmaceutic adjuvant is medicinal rank, and meets national standard.On this basis, draft the quality determining method of this Chewable Tablets of Chinese traditional medicine.
The present invention adopts coprecipitation with medicine material inclusion agents enclose, in the enclose powder, add suitable pharmaceutic adjuvant again, make chewable tablet, covered the uncomfortable taste that medicine material has, good, the taking convenience of mouthfeel not only, and increased the dissolubility of medicine material, improved mouldability and the quality stability of preparation.Medicine is by chewing, and its effective ingredient absorbs rapidly by oral mucosa or hypoglossis mucous membrane, and bioavailability is high.Method of quality control precision of the present invention is high, favorable reproducibility, and the response rate is high, has improved quality standard, can effectively guarantee the quality of the pharmaceutical preparations.
Particularly, Adopts measure of the present invention is as follows:
Chewable Tablets of Chinese traditional medicine of the present invention is made by crude drug and the pharmaceutic adjuvant of following percentage by weight:
Wherein, the main effective ingredient of described Radix Scutellariae extract is baicalin; The weight percent content of baicalin is for being not less than 70% in its described Radix Scutellariae extract;
Again wherein, the main effective ingredient of described Fructus Gardeniae extract is jasminoidin; The weight percent content of jasminoidin is for being not less than 50% in its described Fructus Gardeniae extract.
In above-mentioned Chewable Tablets of Chinese traditional medicine, described inclusion agents is used for the enclose medicine material to cover its uncomfortable taste, is selected from alpha-cyclodextrin, beta-schardinger dextrin-, gamma-cyclodextrin, Hydroxyproply-α-cyclodextrin, HP-β-CD, hydroxypropyl-gamma-cyclodextrin, methyl-beta-schardinger dextrin-, carboxymethyl-beta-cyclodextrin or one chlorotriazine-beta-schardinger dextrin-one or more.
In above-mentioned Chewable Tablets of Chinese traditional medicine, described filler is as diluent, is selected from lactose, sorbitol, mannitol, xylitol, microcrystalline Cellulose, dextrin, sucrose, fructose, glucose, soluble starch or the Mel one or more; Flowability when described lubricant is used for increasing the preparation tabletting is selected from magnesium stearate, micropowder silica gel, Pulvis Talci, Polyethylene Glycol or the microcrystalline Cellulose one or more; Described correctives is used for the mouthfeel of corrigent raw material, is selected from that sucrose, A Siba are sweet, in stevioside, acesulfame potassium, cyclamate, glycyrrhizin, chocolate, organic acid, acylate or the essence one or more; Described binding agent is used for increasing the bonding force between the medicine, is selected from the pressed powder of the pressed powder of gelatin, Resina persicae, tragcanth, xanthan gum, propolis, carrageenan, guar gum, agar, arabic gum, sodium alginate, pectin, Semen Lini glue, the polysaccharide that condenses, pulullan, gellan gum, propylene glycol alginate, locust bean gum or solution, Konjac glucomannan or in solution, ethanol, polyglycol solution, polyvinylpyrrolidonesolution solution or the cellulose derivative alcoholic solution one or more; Described disintegrating agent is used for realizing the disintegrate of chewable tablet, accelerate the absorption of active constituents of medicine, be selected from one or more in sodium carboxymethyl cellulose, crospolyvinylpyrrolidone, low-substituted hydroxypropyl cellulose, Sodium Hydroxymethyl Stalcs, cross-linking sodium carboxymethyl cellulose, hydroxypropyl starch or the micropowder silica gel.
Preferably, Chewable Tablets of Chinese traditional medicine of the present invention is made by crude drug and the pharmaceutic adjuvant of following percentage by weight:
Wherein, the main effective ingredient of described Radix Scutellariae extract is baicalin; The weight percent content of baicalin is for being not less than 70% in its described Radix Scutellariae extract;
Again wherein, the main effective ingredient of described Fructus Gardeniae extract is jasminoidin; The weight percent content of jasminoidin is for being not less than 50% in its described Fructus Gardeniae extract.
The sheet of Chewable Tablets of Chinese traditional medicine of the present invention heavily is 100～1000 mg.
The preparation method of Chewable Tablets of Chinese traditional medicine of the present invention comprises the steps: Radix Scutellariae extract and Fructus Gardeniae extract are dissolved with the ethanol slight fever; Under 80 ℃ of conditions the inclusion agents water is made saturated solution; Under the stirring condition medicine material alcoholic solution slowly is added in the inclusion agents saturated solution, stopped heating behind constant temperature stirring 1～2 h, continue to be stirred to room temperature, get white suspension, cold preservation 72～120 h, sucking filtration, precipitate washing with alcohol 2～4 times, 40～60 ℃ of drying under reduced pressure are pulverized, and obtain the medicine material clathrate; With filler, correctives and disintegrating agent mix homogeneously, add the medicine material clathrate, mixing, with 15%～30% binding agent, 60%～80% alcoholic solution soft material processed, 20～40 mesh sieves are granulated, 40～60 ℃ of dryings; Dried granule adds the lubricant mixing with 20～40 mesh sieve granulate, tabletting, and quality inspection, packing namely gets Chewable Tablets of Chinese traditional medicine.
In the preparation method of above-mentioned Chewable Tablets of Chinese traditional medicine, the preparation method of Radix Scutellariae extract comprises the steps: to get Radix Scutellariae and smashes, add in 10 times of amount boiling water, decoct 3 times, 2 h/ time, collecting decoction, centrifugal, the centrifugal liquid concentrating under reduced pressure becomes every 1ml to contain the medicinal liquid (the room temperature relative density is about 1.15) of 0.25g crude drug, uses 2mol.L
-1Hydrochloric acid solution is transferred pH to 2, and 80 ℃ of insulation 60min leave standstill 12h, and collecting precipitation and being suspended in waits in the water gaging, transfers pH to 7 with 40% sodium hydroxide solution, adds ethanol, make to contain the alcohol amount and reach 50%, and fully stirring, filtration, filtrate is used 2mol.L
-1Hydrochloric acid solution is transferred pH to 2, and 80 ℃ of insulation 60min leave standstill 12h, and it is 4.0 that collecting precipitation also is washed till pH with 50% ethanol, and drying under reduced pressure namely gets Radix Scutellariae extract.
In the preparation method of above-mentioned Chewable Tablets of Chinese traditional medicine, the preparation method of Fructus Gardeniae extract comprises the steps: Fructus Gardeniae extract: the preparation method of described Fructus Gardeniae extract, may further comprise the steps: get Fructus Gardeniae and smash, add 8 times of amounts of 70% ethanol, atmospheric pressure reflux 2 times, each 1.5 h, merge extractive liquid,, centrifugal, the centrifugal liquid Recycled ethanol, concentrating under reduced pressure, water are made the medicinal liquid (the room temperature relative density is about 1.12) that every 1ml contains the 0.5g crude drug, centrifugal, centrifugal liquid is adsorbed with the HPD450 macroporous adsorbent resin bed that is equivalent to 2 times of crude drug amounts, and flow velocity is 0.5BV/h, adsorbs complete rear with 4BV 70% ethanol elution, flow velocity 2BV/h, eluent filters, Recycled ethanol, concentrating under reduced pressure, drying namely gets Fructus Gardeniae extract.
The quality determining method of Chewable Tablets of Chinese traditional medicine of the present invention comprises the steps:
[discriminating]
(1) get 1～4 of this product, grind, add 30～100% methanol, 20～100ml, 25 ℃ of ultrasonic 20～40min filter, and subsequent filtrate is as need testing solution, or get subsequent filtrate 1～5ml evaporate to dryness, and residue adds methanol 1～2ml makes dissolving, as need testing solution; Get the baicalin reference substance an amount of, add 30～100% methanol and make the solution that concentration is 0.5～3mg/ml, in contrast product solution.Test according to an appendix VI of Chinese Pharmacopoeia version in 2010 B thin layer chromatography, draw each 2～10 μ l of above-mentioned need testing solution and reference substance solution, put respectively in same take the carboxymethylcellulose sodium solution that contains 4% sodium acetate on the silica gel g thin-layer plate of binding agent, take ethyl acetate-butanone of volume ratio 5:3:1:1-formic acid-water as developing solvent, pre-equilibration 30min launches, and takes out, dry, spray is with 1% ferric chloride alcoholic solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, aobvious one identical dirty-green speckle.
(2) get 1～10 of this product, grind, add 30～100% methanol, 20～100ml, 25 ℃ of ultrasonic 20～40min filter, and subsequent filtrate is as need testing solution, or get subsequent filtrate 1～5ml evaporate to dryness, and residue adds methanol 1～2ml makes dissolving, as need testing solution; Get the jasminoidin reference substance an amount of, add 30～100% methanol and make the solution that concentration is 2～10mg/ml, in contrast product solution.Test according to an appendix VI of Chinese Pharmacopoeia version in 2010 B thin layer chromatography, draw each 2～10 μ l of above-mentioned need testing solution and reference substance solution, put respectively in same take the carboxymethylcellulose sodium solution that contains 4% sodium acetate on the silica gel g thin-layer plate of binding agent, ethyl acetate-acetone take volume ratio as 5:5:1:1-formic acid-water is developing solvent, launch, take out, dry, spray is heated to the speckle colour developing at 110 ℃ clear with sulphuric acid ethanol (5 → 10) solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, the speckle of aobvious same color;
[inspection] this product should meet the every regulation under an appendix I of Chinese Pharmacopoeia version in 2010 the D rules of preparations tablet item.
[assay] is according to an appendix VI of Chinese Pharmacopoeia version in 2010 D high effective liquid chromatography for measuring.
(1) baicalin
Chromatographic condition and system suitability: be filler with octadecylsilane chemically bonded silica, 30 ℃ of column temperatures, take the methanol-water-phosphoric acid of volume ratio 47:53:0.2 as mobile phase, flow velocity is 1ml/min, the detection wavelength is 280nm, and theoretical cam curve is calculated by the baicalin peak should be not less than 2500;
The preparation of reference substance solution: it is an amount of that precision takes by weighing the baicalin reference substance, adds 30～100% methanol and make the solution that concentration is 30～150 μ g/ml, and get final product;
The preparation of need testing solution: get 1～4 of this product, grind, accurately weighed, put in 10～100ml measuring bottle, add 30～100% methanol to scale, 25 ℃ of ultrasonic 20～40min let cool, add 30～100% methanol to scale, 0.45 μ m filtering with microporous membrane is got subsequent filtrate 1～5ml and is put in 5～50ml measuring bottle, adds 30～100% methanol to scale, shake up, and get final product;
Algoscopy: precision is drawn reference substance solution and each 2～15 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product;
(2) jasminoidin
Chromatographic condition and system suitability: be filler with octadecylsilane chemically bonded silica, 30 ℃ of column temperatures, the acetonitrile-water take volume ratio as 15:85 is mobile phase, flow velocity is 1ml/min, the detection wavelength is 238nm, and theoretical cam curve is calculated by the jasminoidin peak should be not less than 1500;
The preparation of reference substance solution: it is an amount of that precision takes by weighing the jasminoidin reference substance, adds 30～100% methanol and make the solution that concentration is 10～100 μ g/ml, and get final product;
The preparation of need testing solution: get 1～10 of this product, grind, accurately weighed, put in 10～100ml measuring bottle, add 30～100% methanol to scale, 25 ℃ of ultrasonic 30min let cool, add 30～100% methanol to scale, 0.45 μ m filtering with microporous membrane is got subsequent filtrate 1～5ml and is put in 5～50ml measuring bottle, adds 30～100% methanol to scale, shake up, and get final product;
Algoscopy: precision is drawn reference substance solution and each 2～15 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
Chewable Tablets of Chinese traditional medicine of the present invention is compared with conventional tablet has following advantage:
(1) absorption is faster, need not disintegrating procedue, good dispersing state, and drug-eluting speed is fast, absorbs rapidly.
(2) drug effect is stronger, can directly act on respiratory tract, has greatly improved bioavailability, and curative effect is better.
(3) scope of application is wider, and taking convenience need not with mixing in water for oral taking or takes; Absorb by oral mucosa after chewing, mouthfeel is good, can reduce the gastrointestinal untoward reaction, and compliance is good, especially is fit to old man, child and the patient of difficulty that swallows; Also can be made into the sugar-free type that is conducive to diabetic to take.
The usage of Chewable Tablets of Chinese traditional medicine of the present invention and consumption depend primarily on patient's the factors such as age, body constitution and state of an illness weight, and concrete condition strictly complies with the doctor's request.Take by the preparation of the present invention of the described method preparation of the embodiment of the invention 1 as example, its usage and consumption are oral administration, each serving with 2, every day 3 times, whole disease is namely ended.
Chewable Tablets of Chinese traditional medicine of the present invention has good curative effect to treatment upper respiratory tract infection, for illustrating its therapeutical effect, we have done a large amount of experimentatioies, and the below adopts the experimental example of Chewable Tablets of Chinese traditional medicine pharmacodynamic study of the present invention to be used for further specifying, and concrete experimental data is as follows:
1. experiment material
(1) medicine: test used medicine Chewable Tablets of Chinese traditional medicine of the present invention, make by crude drug and the pharmaceutic adjuvant of following percentage by weight:
The sheet of every Chewable Tablets of Chinese traditional medicine is 0.45g heavily, is equivalent to the 4g crude drug; Ribavirin tablet, Meidakang Pharmaceutical Co., Ltd., Sichuan Prov.; SHUANGHUANGLIAN KOUFUYE, He'nan Zhulin Zhongsheng Pharmaceutical Industry Co. Ltd; Aspirin, Astra (Wuxi) pharmaceutical Co. Ltd; The tramadol hydrochloride capsule, the safe company limited of German Glan.
(2) Strain: influenza A virus A/PR/8/34,98-76, Virology Inst., China Academy of Preventive Medicine Sciences are prevented in Influenza B virus B/ capital.
(3) bacterial strain: reference culture: staphylococcus aureus (25923), escherichia coli (25922), Ministry of Public Health microbial identification institute; Table staphylococcus, middle staphylococcus, dissolving staphylococcal bacteria, Bacillus alcaligenes, very become bacillus, acinetobacter calcoaceticus, group B streptococcus, staphylococcus aureus (standard), escherichia coli (standard), Hough Leah bacillus, Bacillus proteus, the abnormal bacillus of plate, citric acid enterobacteria, staphylococcus hominis and Diplococcus pneumoniae, clinical isolates strain.
(4) animal: KM kind white mice, body weight 18～22g; The SD rat, 180～220g; Rabbit, 2.2～2.4kg, male and female half and half, Chongqing Institute of Chinese Medicine Experimental Animal Center.
(5) reagent: dimethylbenzene, Solution on Chemical Reagents in Shanghai purchasing and supply station; Glacial acetic acid, the Nanjing chemical reagent factory; Endotoxin, U.S. Sigma company; Dry yeast, Hubei Angel Yeast Co.,Ltd.
2 test methods and result
Test according to content described below respectively.The quantitative response data represent with mean+SD, and the qualitative response data represent with percentage rate, adopt respectively t check, X
2Statistical procedures is carried out in check.
(1) antivirus action
1. to the protective effect of first type or Influenza B virus infecting mouse
Get 120 of KM kind mices, be divided at random 6 groups, 20 every group.60min after the first administration, except Normal group, all the other respectively organize mice under ether light anaesthesia state, infect every Mus 30 μ l(20 LD to the mice collunarium with first type or the Influenza B virus allantoic fluid of hemagglutination test more than 640
50Challenging dose).Each group is pressed the dosage gastric infusion 20ml/kg shown in the table 1, every day 1 time, continuous 5 days, Normal group, model group gavage equal-volume distilled water.Day by day observe morbidity and death condition after zoogenetic infection and the administration, record the death toll in 14 days.The results detailed in Table 1.
The protective effect of table 1 pair first type or Influenza B virus infecting mouse (
, n=20)
Annotate: compare with model group: * p＜0.05, * * p＜0.01, * * * p＜0.001.
As can be seen from Table 1, three dosage of medicine of the present invention all can improve the survival rate of first type and Influenza B virus infecting mouse to some extent, prolong the time-to-live of first type and Influenza B virus infecting mouse, wherein, the effect of 4 g (crude drug)/kg dosage and 8 g (crude drug)/kg dosage is obvious, compare with model group, significance or utmost point significant difference (p＜0.05 or p＜0.01) are arranged.
2. on the impact of first type or Influenza B virus Lung Index of mice infected by Influenza virus
Get 60 of KM kind mices, be divided at random 6 groups, 10 every group.Grouping, modeling and medication are with above-mentioned experiment 1..3h after the last administration, each is organized mice and weighs, and takes off cervical vertebra and puts to death, dissect, observe pulmonary lesion, get lung and weigh, calculate lung index [heavy (the mg)/body weight (g) of=lung] and lung index [=(model group lung Mean value of index-treatment group lung Mean value of index)/model group lung Mean value of index * 100%].The results detailed in Table 2.
Table 2 on the impact of first type or Influenza B virus Lung Index of mice infected by Influenza virus (
, n=10)
Annotate: compare with normal group: △ △ p＜0.01, △ △ △ p＜0.001; Compare with model group: * p＜0.05, * * p＜0.01, * * * p＜0.001.
As can be seen from Table 2, model group mouse lung index obviously raises, and compares with Normal group, and utmost point significance or significant differences (p＜0.01 or p＜0.001) are arranged; Three dosage of medicine of the present invention all can reduce the lung index of first type and Influenza B virus infecting mouse to some extent, wherein, the effect of 4 g (crude drug)/kg and 8 g (crude drug)/kg dosage is obvious, compares with model group, and significant difference (p＜0.05) is arranged.
The result of histopathologic examination shows, mice after first type and Influenza B virus collunarium infect obvious pulmonary inflammatory lesion can occur, and main manifestations is bronchitis and interstitial pneumonia.Three dosage of medicine of the present invention all can reverse above-mentioned pathological changes to some extent.
3. brief summary
The experimental result of table 1～2 shows, medicine Chewable Tablets of Chinese traditional medicine of the present invention has obvious antivirus action.
(2) antibacterial action
1. vitro antibacterial activity
Get each bacterial strain shown in the table 3 a little, be inoculated in the broth bouillon, cultivate 18h, prepare bacterium liquid with normal saline for 37 ℃.After drug solution of the present invention and the SHUANGHUANGLIAN KOUFUYE sterilization, get an amount of and agar culture medium mixing, prepare successively serial pastille plate by the drug level shown in the table 3.Make a call to 3 holes at the pastille plate with the aseptic steel ring of 6mm, it is 10 that above-mentioned bacterium liquid 0.1ml(bacteria containing amount is injected in every hole
-5CFU/ml), cultivate 18～20h for 37 ℃, examine and record the growing state of antibacterial, analyze the minimum inhibitory concentration (MIC) of judging medicine.The results detailed in Table 3.
The In-vitro Inhibitory Effect (n=2) of table 3 pair serial antibacterial
As can be seen from Table 3, medicine his-and-hers watches staphylococcus of the present invention, staphylococcus aureus, middle staphylococcus, dissolving staphylococcal bacteria, Bacillus alcaligenes, escherichia coli, very become bacillus, acinetobacter calcoaceticus, group B streptococcus, staphylococcus aureus (standard), escherichia coli (standard), Hough Leah bacillus, Bacillus proteus, the abnormal bacillus of plate, citric acid enterobacteria, staphylococcus hominis and Diplococcus pneumoniae and have stronger inhibitory action, MIC is 0.02～0.36 g (crude drug)/ml.
2. to the protective effect of staphylococcus aureus or Diplococcus pneumoniae infecting mouse
Get 120 of KM kind mices, be divided at random 6 groups, 20 every group.Each group is pressed the dosage gastric infusion 20ml/kg shown in the table 4, every day 1 time, continuous 5 days, Normal group, model group gavage equal-volume distilled water.60min after the administration in the 3rd day, except Normal group, (bacteria containing amount is 1 LD for lumbar injection staphylococcus aureus or Diplococcus pneumoniae culture fluid
50) 0.5ml/ only.Morbidity and death condition after observation zoogenetic infection and the administration record the death toll in 7 days.The results detailed in Table 4.
The protective effect of table 4 pair staphylococcus aureus or Diplococcus pneumoniae infecting mouse (
, n=20)
Annotate: compare with model group: * p＜0.05, * * p＜0.01, * * * p＜0.001.
As can be seen from Table 4, three dosage of medicine of the present invention all can improve the survival rate of staphylococcus aureus or Diplococcus pneumoniae infecting mouse to some extent, but not statistically significant, prolong the time-to-live of staphylococcus aureus or Diplococcus pneumoniae infecting mouse, wherein, the effect of 8 g (crude drug)/kg dosage is obvious, compares with model group, and significant difference (p＜0.05) is arranged.
3. brief summary
The experimental result of table 3～4 shows, medicine Chewable Tablets of Chinese traditional medicine of the present invention has certain antibacterial action.
(3) antiinflammatory action
1. Dichlorodiphenyl Acetate causes the impact that the mice capillary permeability increases
Get 50 of KM kind mices, be divided at random 5 groups, 10 every group.Each group is pressed the dosage gastric infusion 20ml/kg shown in the table 5, every day 1 time, for three days on end, model group gavage equal-volume distilled water.45min after the last administration, tail vein injection 0.5% azovan blue normal saline solution 0.1ml/10g, retinue lumbar injection 0.6% acetic acid 0.1ml/10g, behind the 20min, put to death mice, open the abdominal cavity, repeatedly wash the abdominal cavity three times with the 5ml normal saline, collect cleaning mixture, the centrifugal 5min of 1000rpm, ultraviolet spectrophotometer 590nm place measures trap (OD value).The results detailed in Table 5.
Table 5 Dichlorodiphenyl Acetate cause the impact that the mice capillary permeability increases (
, n=10)
| Group | Dosage [g (crude drug)/kg] | Trap (OD value) |
| Model | - | 0.215±0.053 |
| Aspirin | 0.6 | 0.135±0.047** |
| Medicine of the present invention | 8 | 0.137±0.045** |
| Medicine of the present invention | 4 | 0.148±0.076* |
| Medicine of the present invention | 2 | 0.177±0.082 |
Annotate: compare with model group: * p＜0.05, * * p＜0.01, * * * p＜0.001.
As can be seen from Table 5, three dosage of medicine of the present invention all can reduce the mice capillary permeability increase that acetic acid causes to some extent, wherein, the effect of 4 g (crude drug)/kg and 8 g (crude drug)/kg dosage is obvious, compare with model group, significance or utmost point significant difference (p＜0.05 or p＜0.01) are arranged.
2. xylol causes the antiinflammatory action of mice ear
Get 50 of KM kind mices, be divided at random 5 groups, 10 every group.Each group is pressed the dosage gastric infusion 20ml/kg shown in the table 6, every day 1 time, for three days on end, model group gavage equal-volume distilled water.45min after the last administration, the mouse right ear two sides only is coated with dimethylbenzene 0.05ml/, and left ear is not coated with.Put to death mice behind the 45min, lay disk in the ears same area respectively, weigh, calculate swelling (=auris dextra weight-left ear weight), inhibitory rate of intumesce [=(model group swelling average-administration group swelling average)/model group swelling average * 100%].The results detailed in Table 6.
Table 6 xylol cause mice ear antiinflammatory action (
, n=10)
| Group | Dosage [g (crude drug)/kg] | Auricle swelling degree (mg) | Inhibitory rate of intumesce (%) |
| Model | - | 0.0181±0.0057 | |
| Aspirin | 0.6 | 0.0051±0.0039*** | 71.82 |
| Medicine of the present invention | 8 | 0.0096±0.0061** | 46.96 |
| Medicine of the present invention | 4 | 0.0114±0.0056* | 37.02 |
| Medicine of the present invention | 2 | 0.0165±0.0049 | 8.84 |
Annotate: compare with model group: * p＜0.05, * * p＜0.01, * * * p＜0.001.
As can be seen from Table 6, three dosage of medicine of the present invention all can reduce the mice ear that dimethylbenzene causes to some extent, wherein, the effect of 4 g (crude drug)/kg and 8 g (crude drug)/kg dosage is obvious, compare with model group, significance or utmost point significant difference (p＜0.05 or p＜0.01) are arranged.
3. brief summary
The experimental result of table 5～6 shows, medicine Chewable Tablets of Chinese traditional medicine of the present invention stimulates the inflammatory reaction that causes to have certain antagonism to chemical substance.
(4) analgesic activity
1. Dichlorodiphenyl Acetate causes the impact of mice pain
Get 50 of KM kind mices, be divided at random 5 groups, 10 every group.Each group is pressed the dosage gastric infusion 20ml/kg shown in the table 7, model group gavage equal-volume distilled water.45min after the administration, lumbar injection 0.6% acetum 0.1ml/10g, observe the writhing response number of times (abdominal part indent, stretching, extension hind leg, buttocks are raised) that the rear 15min of injection occurs, calculate analgesia percentage rate [=(model group writhing number of times average-administration group writhing number of times average)/model group writhing number of times average * 100%].The results detailed in Table 7.
Table 7 Dichlorodiphenyl Acetate cause mice pain impact (
, n=10)
| Group | Dosage [g (crude drug)/kg] | The writhing number of times | Analgesia percentage rate (%) |
| Model | - | 35.1±6.9 | - |
| Tramadol hydrochloride | 0.133 | 21.7±11.1* | 38.18 |
| Medicine of the present invention | 8 | 26.9±10.6 | 23.36 |
| Medicine of the present invention | 4 | 28.6±9.8 | 18.52 |
| Medicine of the present invention | 2 | 31.5±11.4 | 10.26 |
Annotate: compare with model group: * p＜0.05, * * p＜0.01, * * * p＜0.001.
As can be seen from Table 7, three dosage of medicine of the present invention all can reduce the writhing number of times of acetic acid induced pain mice to some extent, but compare with model group, there was no significant difference (p〉0.05).
2. thermostimulation is caused the impact of mice pain
KM kind female mice is placed on the hot plate (55 ± 0.5 ℃ water-bath preheating 10 minutes), 1/time, with mice from being put on the hot plate to occurring licking the required time of metapedes (second) as the pain threshold of this Mus.Select the mice of pain threshold in 5～30 seconds scopes to be used for experiment, the meansigma methods that pain threshold is got two subnormal pain thresholds before its medicine.Get 50 of mices, be divided at random 5 groups, 10 every group.Each group is pressed the dosage gastric infusion 20ml/kg shown in the table 8, model group gavage equal-volume distilled water.45min after the administration by the time point determining mice pain threshold of setting, improves the diversity that percentage rate comes the comparative drug effect with the threshold of pain.The results detailed in Table 8.
Table 8 on thermostimulation cause mice pain impact (
, n=10)
Annotate: compare with model group: * p＜0.05, * * p＜0.01, * * * p＜0.001.
As can be seen from Table 8, three dosage of medicine of the present invention all can improve the pain threshold (threshold of pain raising percentage rate) of thermostimulation induced pain mice to some extent, and wherein, the effect of 8 g (crude drug)/kg dosage is obvious, compare with model group, significant difference (p＜0.05) is arranged.
3. brief summary
The experimental result of table 7～8 shows, medicine Chewable Tablets of Chinese traditional medicine of the present invention stimulates without obvious analgesic activity chemical substance, but physical stimulation is had analgesic activity.
(5) refrigeration function
1. dry yeast is caused the impact of heating rat
Rat fasting 12 hours before the experiment freely drink water, tests and surveys body temperature 2 times the same day, and every 2 hours once, the selection temperature difference is no more than 50 of 0.3 ℃, the rat of body temperature in 36.6 ℃～38.3 ℃ scopes, is divided at random 5 groups, 10 every group.Each group is pressed the dosage gastric infusion 20ml/kg shown in the table 9, model group gavage equal-volume distilled water.Then back subcutaneous injection 15% dry yeast suspension 10ml/kg immediately after the administration surveys the anus temperature at 1h, 2h, 4h, 6h, 8h, 10h respectively, obtains each time point body temperature with respect to the changing value of normal body temperature.The results detailed in Table 9.
Table 9 on dry yeast cause the heating rat impact (
, n=10)
Annotate: compare with model group: * p＜0.05, * * p＜0.01.
As can be seen from Table 9, three dosage of medicine of the present invention all can reduce the body temperature (or Δ T) that dry yeast causes the heating rat to some extent, wherein, 3.2 the effect of g (crude drug)/kg and 6.4 g (crude drug)/kg dosage 4h, 6h after administration is obvious, compare with model group, significant difference (p＜0.05) is arranged.
2. induced by endotoxin causes the impact of fever in rabbit
Test front 2 day set time and measure rabbit anus temperature once, get the rabbit in 38.5 ℃～39.5 ℃ scopes, behind the auricular vein endotoxin injection 1h, select 30 of the fever in rabbit of the temperature difference above 1.0 ℃, divide at random 5 groups, 6 every group.Each group is pressed the dosage gastric infusion 1ml/kg shown in the table 10, model group gavage equal-volume distilled water.1h, 2h, 3h, 4h, 5h, 6h survey the anus temperature after the administration, obtain each time point body temperature with respect to the changing value of normal body temperature.The results detailed in Table 10.
Table 10 induced by endotoxin cause fever in rabbit impact (
, n=6)
Annotate: compare with model group: * p＜0.05, * * p＜0.01.
As can be seen from Table 10, three dosage of medicine of the present invention all can reduce the body temperature (or Δ T) that endotoxin causes fever in rabbit to some extent, and wherein, the effect of 3.2 g (crude drug)/kg dosage 2h, 3h after administration is obvious, compare with model group, significant difference (p＜0.05) is arranged.
3. brief summary
The experimental result of table 9～10 shows, medicine Chewable Tablets of Chinese traditional medicine of the present invention has certain refrigeration function.
3 conclusion (of pressure testing)s
The test of pesticide effectiveness confirms, Chewable Tablets of Chinese traditional medicine of the present invention has first type and/or Influenza B virus, streptococcus pneumoniae, pneumobacillus to be killed or inhibitory action significantly, and has the effects such as analgesic, antiinflammatory, analgesia.Compare with existing commercial preparation, have that raw material sources are extensive, preparation technique is advanced, the many target spots of drug action, multi-level, safety coefficient is large, and taking dose is little, and dosage form meets clinical needs.
The specific embodiment
Below by embodiment, the present invention is further described, should be understood that following embodiment only is used for explanation the present invention, and unrestricted the present invention.
Embodiment 1
[prescription]
Crude drug and the pharmaceutic adjuvant of above-mentioned weight are made 1000 Chewable Tablets of Chinese traditional medicines altogether.
[method for making] dissolves Radix Scutellariae extract and Fructus Gardeniae extract with an amount of ethanol slight fever; Preparation beta-schardinger dextrin-saturated aqueous solution under 80 ℃ of conditions; Under the stirring condition medicine material alcoholic solution is slowly added in the beta-schardinger dextrin-saturated aqueous solution, constant temperature stirs stopped heating after 1 hour, continues to be stirred to room temperature, get white suspension, cold preservation 72 hours, sucking filtration, precipitate washing with alcohol 2 times, 60 ℃ of drying under reduced pressure are pulverized; With lactose, xylitol, mannitol, soluble starch and sodium carboxymethyl cellulose mix homogeneously, add the medicine material clathrate, mixing, with 15% polyvinylpyrrolidone, 80% alcoholic solution soft material processed, 20 mesh sieves are granulated, 60 ℃ of drying under reduced pressure; Dried granule adds the magnesium stearate mixing with 20 mesh sieve granulate, tabletting, and quality inspection, packing, and get final product.
[discriminating]
(1) get 1 of this product, grind, add 30～100% methanol 50ml, 25 ℃ of ultrasonic 20min filter, and get subsequent filtrate as need testing solution.Get the baicalin reference substance an amount of, add methanol and make the solution that concentration is 2.4mg/ml, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 B) test, draw each 2 μ l of above-mentioned need testing solution and reference substance solution, put respectively in same take the carboxymethylcellulose sodium solution that contains 4% sodium acetate on the silica gel g thin-layer plate of binding agent, take ethyl acetate-butanone-formic acid-water (volume ratio is as 5:3:1:1) as developing solvent, pre-equilibration 30min launches, and takes out, dry, spray is with 1% ferric chloride alcoholic solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, aobvious one identical dirty-green speckle.
(2) get 5 of this product, grind, add 30～100% methanol 50ml, 25 ℃ of ultrasonic 20min filter, and get subsequent filtrate 1.7ml evaporate to dryness, and residue adds methanol 1ml makes dissolving, as need testing solution.Get the jasminoidin reference substance an amount of, add 30～100% methanol and make the solution that concentration is 6.5mg/ml, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 B) test, draw each 3 μ l of above-mentioned need testing solution and reference substance solution, put respectively in same take the carboxymethylcellulose sodium solution that contains 4% sodium acetate on the silica gel g thin-layer plate of binding agent, take ethyl acetate-acetone-formic acid-water (volume ratio is as 5:5:1:1) as developing solvent, launch, take out, dry, spray is heated to the speckle colour developing at 110 ℃ clear with sulphuric acid ethanol (5 → 10) solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, the speckle of aobvious same color.
[inspection] this product should meet every regulation under the rules of preparations tablet item (" an appendix I of Chinese pharmacopoeia version in 2010 D).
[assay]
Measure according to high performance liquid chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 D).
(1) baicalin
Chromatographic condition and system suitability: be filler with octadecylsilane chemically bonded silica, 30 ℃ of column temperatures, methanol-water-phosphoric acid (volume ratio is 47:53:0.2) is mobile phase, flow velocity is 1ml/min, the detection wavelength is 280nm, and theoretical cam curve is calculated by the baicalin peak should be not less than 2500.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the baicalin reference substance, adds 30～100% methanol and make the solution that concentration is 140 μ g/ml, and get final product.
The preparation of need testing solution: get 1 of this product, grind, accurately weighed, put in the 50ml measuring bottle, add 30～100% methanol to scale, 25 ℃ of ultrasonic 20min let cool, add 30～100% methanol to scale, 0.45 μ m filtering with microporous membrane is got subsequent filtrate 2.8ml and is put in the 50ml measuring bottle, adds 30～100% methanol to scale, shake up, and get final product.
Algoscopy: precision is drawn reference substance solution and each 4 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The result: this product content of baicalin is the 160mg/ sheet.
(2) jasminoidin
Chromatographic condition and system suitability: be filler with octadecylsilane chemically bonded silica, 30 ℃ of column temperatures, acetonitrile-water (volume ratio is 15:85) is mobile phase, flow velocity is 1ml/min, the detection wavelength is 238nm, and theoretical cam curve is calculated by the jasminoidin peak should be not less than 1500.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the jasminoidin reference substance, adds 30～100% methanol and make the solution that concentration is 50 μ g/ml, and get final product.
The preparation of need testing solution: get 2 of this product, grind, accurately weighed, put in the 100ml measuring bottle, add 30～100% methanol to scale, 25 ℃ of ultrasonic 20min let cool, add 30～100% methanol to scale, 0.45 μ m filtering with microporous membrane is got subsequent filtrate 1.6ml and is put in the 25ml measuring bottle, adds 30～100% methanol to scale, shake up, and get final product.
Algoscopy: precision is drawn reference substance solution and each 6 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The result: this product Determination of Gardenoside is the 48mg/ sheet.
Embodiment 2
[prescription]
Crude drug and the pharmaceutic adjuvant of above-mentioned weight are made 1000 Chewable Tablets of Chinese traditional medicines altogether.
[method for making] dissolves Radix Scutellariae extract and Fructus Gardeniae extract with an amount of ethanol slight fever; Preparation beta-schardinger dextrin-saturated aqueous solution under 80 ℃ of conditions; Under the stirring condition medicine material alcoholic solution is slowly added in the beta-schardinger dextrin-saturated aqueous solution, constant temperature stirs stopped heating after 1.5 hours, continues to be stirred to room temperature, get white suspension, cold preservation 84 hours, sucking filtration, precipitate washing with alcohol 3 times, 50 ℃ of drying under reduced pressure are pulverized; With lactose, xylitol, mannitol, soluble starch and sodium carboxymethyl cellulose mix homogeneously, add the medicine material clathrate, mixing, with 20% polyvinylpyrrolidone, 70% alcoholic solution soft material processed, 30 mesh sieves are granulated, 50 ℃ of drying under reduced pressure; Dried granule adds the magnesium stearate mixing with 30 mesh sieve granulate, tabletting, and quality inspection, packing, and get final product.
[discriminating]
(1) get 1 of this product, grind, add 70% methanol 50ml, 25 ℃ of ultrasonic 40min filter, and get subsequent filtrate as need testing solution.Get the baicalin reference substance an amount of, add 70% methanol and make the solution that concentration is 1.2mg/ml, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 B) test, draw each 4 μ l of above-mentioned need testing solution and reference substance solution, remaining step is differentiated with embodiment 1[] (1) lower corresponding contents.
(2) get 6 of this product, grind, add 70% methanol 50ml, 25 ℃ of ultrasonic 40min filter, and get subsequent filtrate 2.4ml evaporate to dryness, and residue adds 70% methanol 1ml makes dissolving, as need testing solution.Get the jasminoidin reference substance an amount of, add 70% methanol and make the solution that concentration is 5.5mg/ml, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 B) test, draw each 4 μ l of above-mentioned need testing solution and reference substance solution, remaining step is differentiated with embodiment 1[] (2) lower corresponding contents.
[inspection] checks with embodiment 1[] a lower corresponding contents.
[assay]
(1) baicalin method foundation, chromatographic condition and system suitability are with embodiment 1[assay] (1) lower corresponding contents.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the baicalin reference substance, adds 70% methanol and make the solution that concentration is 70 μ g/ml, and get final product.
The preparation of need testing solution: get 1 of this product, grind, accurately weighed, put in the 50ml measuring bottle, add 70% methanol to scale, 25 ℃ of ultrasonic 40min let cool, and add 70% methanol to scale, 0.45 μ m filtering with microporous membrane, get subsequent filtrate 2.8ml and put in the 50ml measuring bottle, add 70% methanol to scale, shake up, and get final product.
Algoscopy: precision is drawn reference substance solution and each 9 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The result: this product content of baicalin is the 80mg/ sheet.
(2) jasminoidin method foundation, chromatographic condition and system suitability are with embodiment 1[assay] (2) lower corresponding contents.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the jasminoidin reference substance, adds 70% methanol and make the solution that concentration is 40 μ g/ml, and get final product.
The preparation of need testing solution: get 1 of this product, grind, accurately weighed, put in the 50ml measuring bottle, add 70% methanol to scale, 25 ℃ of ultrasonic 40min let cool, and add 70% methanol to scale, 0.45 μ m filtering with microporous membrane, get subsequent filtrate 5.0ml and put in the 50ml measuring bottle, add 70% methanol to scale, shake up, and get final product.
Algoscopy: precision is drawn reference substance solution and each 8 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The result: this product Determination of Gardenoside is the 24mg/ sheet.
Embodiment 3
[prescription]
Crude drug and the pharmaceutic adjuvant of above-mentioned weight are made 1000 Chewable Tablets of Chinese traditional medicines altogether.
[method for making] dissolves Radix Scutellariae extract and Fructus Gardeniae extract with an amount of ethanol slight fever; Preparation beta-schardinger dextrin-saturated aqueous solution under 80 ℃ of conditions; Under the stirring condition medicine material alcoholic solution is slowly added in the beta-schardinger dextrin-saturated aqueous solution, constant temperature stirs stopped heating after 2 hours, continues to be stirred to room temperature, get white suspension, cold preservation 96 hours, sucking filtration, precipitate washing with alcohol 4 times, 40 ℃ of drying under reduced pressure are pulverized; With lactose, xylitol, mannitol, soluble starch and sodium carboxymethyl cellulose mix homogeneously, add the medicine material clathrate, mixing, with 25% polyvinylpyrrolidone, 60% alcoholic solution soft material processed, 40 mesh sieves are granulated, 40 ℃ of drying under reduced pressure; Dried granule adds the magnesium stearate mixing with 40 mesh sieve granulate, tabletting, and quality inspection, packing, and get final product.
[discriminating]
(1) get 1 of this product, grind, add 60% methanol 50ml, 25 ℃ of ultrasonic 20min filter, and get subsequent filtrate 1.2ml evaporate to dryness, and residue adds 60% methanol 1ml makes dissolving, as need testing solution.Get the baicalin reference substance an amount of, add 60% methanol and make the solution that concentration is 1.5mg/ml, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 B) test, draw each 3 μ l of above-mentioned need testing solution and reference substance solution, remaining step is differentiated with embodiment 1[] (1) lower corresponding contents.
(2) get 6 of this product, grind, add 60% methanol 50ml, 25 ℃ of ultrasonic 20min filter, and get subsequent filtrate 2.8ml evaporate to dryness, and residue adds 60% methanol 1ml makes dissolving, as need testing solution.Get the jasminoidin reference substance an amount of, add 60% methanol and make the solution that concentration is 6.5mg/ml, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 B) test, draw each 3 μ l of above-mentioned need testing solution and reference substance solution, remaining step is differentiated with embodiment 1[] (2) lower corresponding contents.
[inspection] checks with embodiment 1[] a lower corresponding contents.
[assay]
(1) baicalin method foundation, chromatographic condition and system suitability are with embodiment 1[assay] (1) lower corresponding contents.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the baicalin reference substance, adds 60% methanol and make the solution that concentration is 80 μ g/ml, and get final product.
The preparation of need testing solution: get 1 of this product, grind, accurately weighed, put in the 50ml measuring bottle, add 60% methanol to scale, 25 ℃ of ultrasonic 20min let cool, and add 60% methanol to scale, 0.45 μ m filtering with microporous membrane, get subsequent filtrate 3.1ml and put in the 50ml measuring bottle, add 60% methanol to scale, shake up, and get final product.
Algoscopy: precision is drawn reference substance solution and each 8 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The result: this product content of baicalin is the 80mg/ sheet.
(2) jasminoidin method foundation, chromatographic condition and system suitability are with embodiment 1[assay] (2) lower corresponding contents.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the jasminoidin reference substance, adds 60% methanol and make the solution that concentration is 50 μ g/ml, and get final product.
The preparation of need testing solution: get 1 of this product, grind, accurately weighed, put in the 50ml measuring bottle, add 60% methanol to scale, 25 ℃ of ultrasonic 20min let cool, and add 60% methanol to scale, 0.45 μ m filtering with microporous membrane, get subsequent filtrate 4.5ml and put in the 50ml measuring bottle, add 60% methanol to scale, shake up, and get final product.
Algoscopy: precision is drawn reference substance solution and each 6 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The result: this product Determination of Gardenoside is the 24mg/ sheet.
Embodiment 4
[prescription]
Crude drug and the pharmaceutic adjuvant of above-mentioned weight are made 1000 Chewable Tablets of Chinese traditional medicines altogether.
[method for making] dissolves Radix Scutellariae extract and Fructus Gardeniae extract with an amount of ethanol slight fever; Preparation beta-schardinger dextrin-saturated aqueous solution under 80 ℃ of conditions; Under the stirring condition medicine material alcoholic solution is slowly added in the beta-schardinger dextrin-saturated aqueous solution, constant temperature stirs stopped heating after 1.5 hours, continues to be stirred to room temperature, get white suspension, cold preservation 108 hours, sucking filtration, precipitate washing with alcohol 3 times, 50 ℃ of drying under reduced pressure are pulverized; With lactose, xylitol, mannitol, soluble starch and sodium carboxymethyl cellulose mix homogeneously, add the medicine material clathrate, mixing, with 30% polyvinylpyrrolidone, 70% alcoholic solution soft material processed, 30 mesh sieves are granulated, 50 ℃ of drying under reduced pressure; Dried granule adds the magnesium stearate mixing with 30 mesh sieve granulate, tabletting, and quality inspection, packing, and get final product.
[discriminating]
(1) get 1 of this product, grind, add methanol 25ml, 25 ℃ of ultrasonic 30min filter, and get subsequent filtrate 1.7ml evaporate to dryness, and residue adds methanol 2ml makes dissolving, as need testing solution.Get the baicalin reference substance an amount of, add methanol and make the solution that concentration is 0.9mg/ml, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 B) test, draw each 5 μ l of above-mentioned need testing solution and reference substance solution, remaining step is differentiated with embodiment 1[] (1) lower corresponding contents.
(2) get 4 of this product, grind, add methanol 25ml, 25 ℃ of ultrasonic 30min filter, and get subsequent filtrate 3ml evaporate to dryness, and residue adds methanol 1ml makes dissolving, as need testing solution.Get the jasminoidin reference substance an amount of, add methanol and make the solution that concentration is 4.5mg/ml, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 B) test, draw each 4 μ l of above-mentioned need testing solution and reference substance solution, remaining step is differentiated with embodiment 1[] (2) lower corresponding contents.
[inspection] checks with embodiment 1[] a lower corresponding contents.
[assay]
(1) baicalin method foundation, chromatographic condition and system suitability are with embodiment 1[assay] (1) lower corresponding contents.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the baicalin reference substance, adds methanol and make the solution that concentration is 60 μ g/ml, and get final product.
The preparation of need testing solution: get 1 of this product, grind, accurately weighed, put in the 25ml measuring bottle, add methanol to scale, 25 ℃ of ultrasonic 30min let cool, and add methanol to scale, 0.45 μ m filtering with microporous membrane, get subsequent filtrate 1.2ml and put in the 25ml measuring bottle, add methanol to scale, shake up, and get final product.
Algoscopy: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The result: this product content of baicalin is the 40mg/ sheet.
(2) jasminoidin method foundation, chromatographic condition and system suitability are with embodiment 1[assay] (2) lower corresponding contents.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the jasminoidin reference substance, adds methanol and make the solution that concentration is 30 μ g/ml, and get final product.
The preparation of need testing solution: get 1 of this product, grind, accurately weighed, put in the 25ml measuring bottle, add methanol to scale, 25 ℃ of ultrasonic 30min let cool, and add methanol to scale, 0.45 μ m filtering with microporous membrane, get subsequent filtrate 2ml and put in the 25ml measuring bottle, add methanol to scale, shake up, and get final product.
Algoscopy: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The result: this product Determination of Gardenoside is the 12mg/ sheet.
Embodiment 5
[prescription]
Crude drug and the pharmaceutic adjuvant of above-mentioned weight are made 1000 Chewable Tablets of Chinese traditional medicines altogether.
[method for making] dissolves Radix Scutellariae extract and Fructus Gardeniae extract with an amount of ethanol slight fever; Preparation beta-schardinger dextrin-saturated aqueous solution under 80 ℃ of conditions; Under the stirring condition medicine material alcoholic solution is slowly added in the beta-schardinger dextrin-saturated aqueous solution, constant temperature stirs stopped heating after 2 hours, continues to be stirred to room temperature, get white suspension, cold preservation 120 hours, sucking filtration, precipitate washing with alcohol 4 times, 60 ℃ of drying under reduced pressure are pulverized; With lactose, xylitol, mannitol, soluble starch and sodium carboxymethyl cellulose mix homogeneously, add the medicine material clathrate, mixing, with 25% polyvinylpyrrolidone, 80% alcoholic solution soft material processed, 20 mesh sieves are granulated, 60 ℃ of drying under reduced pressure; Dried granule adds the magnesium stearate mixing with 20 mesh sieve granulate, tabletting, and quality inspection, packing, and get final product.
[discriminating]
(1) get 1 of this product, grind, add 80% methanol 50ml, 25 ℃ of ultrasonic 40min filter, and get subsequent filtrate 1.6ml evaporate to dryness, and residue adds 80% methanol 1ml makes dissolving, as need testing solution.Get the baicalin reference substance an amount of, add 80% methanol and make the solution that concentration is 2.1mg/ml, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 B) test, draw each 2 μ l of above-mentioned need testing solution and reference substance solution, remaining step is differentiated with embodiment 1[] (1) lower corresponding contents.
(2) get 10 of this product, grind, add 80% methanol 50ml, 25 ℃ of ultrasonic 40min filter, and get subsequent filtrate 2.3ml evaporate to dryness, and residue adds 80% methanol 1ml makes dissolving, as need testing solution.Get the jasminoidin reference substance an amount of, add 80% methanol and make the solution that concentration is 8.5mg/ml, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 B) test, draw each 2 μ l of above-mentioned need testing solution and reference substance solution, remaining step is differentiated with embodiment 1[] (2) lower corresponding contents.
[inspection] checks with embodiment 1[] a lower corresponding contents.
[assay]
(1) baicalin method foundation, chromatographic condition and system suitability are with embodiment 1[assay] (1) lower corresponding contents.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the baicalin reference substance, adds 80% methanol and make the solution that concentration is 120 μ g/ml, and get final product.
The preparation of need testing solution: get 1 of this product, grind, accurately weighed, put in the 100ml measuring bottle, add 80% methanol to scale, 25 ℃ of ultrasonic 40min let cool, add 80% methanol to scale, 0.45 μ m filtering with microporous membrane is got subsequent filtrate 4.4ml and is put in the 50ml measuring bottle, adds 80% methanol to scale, shake up, and get final product.
Algoscopy: precision is drawn reference substance solution and each 5 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The result: this product content of baicalin is the 80mg/ sheet.
(2) jasminoidin method foundation, chromatographic condition and system suitability are with embodiment 1[assay] (2) lower corresponding contents.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the jasminoidin reference substance, adds 80% methanol and make the solution that concentration is 70 μ g/ml, and get final product.
The preparation of need testing solution: get 1 of this product, grind, accurately weighed, put in the 100ml measuring bottle, add 80% methanol to scale, 25 ℃ of ultrasonic 40min let cool, add 80% methanol to scale, 0.45 μ m filtering with microporous membrane is got subsequent filtrate 4.2ml and is put in the 25ml measuring bottle, adds 80% methanol to scale, shake up, and get final product.
Algoscopy: precision is drawn reference substance solution and each 4 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The result: this product Determination of Gardenoside is the 24mg/ sheet.
Embodiment 6
[prescription]
Crude drug and the pharmaceutic adjuvant of above-mentioned weight are made 1000 Chewable Tablets of Chinese traditional medicines altogether.
[method for making] dissolves Radix Scutellariae extract and Fructus Gardeniae extract with an amount of ethanol slight fever; Preparation beta-schardinger dextrin-saturated aqueous solution under 80 ℃ of conditions; Under the stirring condition medicine material alcoholic solution is slowly added in the beta-schardinger dextrin-saturated aqueous solution, constant temperature stirs stopped heating after 1 hour, continues to be stirred to room temperature, get white suspension, cold preservation 108 hours, sucking filtration, precipitate washing with alcohol 2 times, 40 ℃ of drying under reduced pressure are pulverized; With lactose, xylitol, mannitol, soluble starch and sodium carboxymethyl cellulose mix homogeneously, add the medicine material clathrate, mixing, with 15% polyvinylpyrrolidone, 60% alcoholic solution soft material processed, 40 mesh sieves are granulated, 40 ℃ of drying under reduced pressure; Dried granule adds the magnesium stearate mixing with 40 mesh sieve granulate, tabletting, and quality inspection, packing, and get final product.
[discriminating]
(1) get 1 of this product, grind, add 40% methanol 50ml, 25 ℃ of ultrasonic 30min filter, and get subsequent filtrate 1.4ml evaporate to dryness, and residue adds 40% methanol 1ml makes dissolving, as need testing solution.Get the baicalin reference substance an amount of, add 40% methanol and make the solution that concentration is 1.8mg/ml, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 B) test, draw each 3 μ l of above-mentioned need testing solution and reference substance solution, remaining step is differentiated with embodiment 1[] (1) lower corresponding contents.
(2) get 8 of this product, grind, add 40% methanol 50ml, 25 ℃ of ultrasonic 30min filter, and get subsequent filtrate 2.5ml evaporate to dryness, and residue adds 40% methanol 1ml makes dissolving, as need testing solution.Get the jasminoidin reference substance an amount of, add 40% methanol and make the solution that concentration is 7.5mg/ml, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 B) test, draw each 3 μ l of above-mentioned need testing solution and reference substance solution, remaining step is differentiated with embodiment 1[] (2) lower corresponding contents.
[inspection] checks with embodiment 1[] a lower corresponding contents.
[assay]
(1) baicalin method foundation, chromatographic condition and system suitability are with embodiment 1[assay] (1) lower corresponding contents.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the baicalin reference substance, adds 40% methanol and make the solution that concentration is 100 μ g/ml, and get final product.
The preparation of need testing solution: get 1 of this product, grind, accurately weighed, put in the 50ml measuring bottle, add 40% methanol to scale, 25 ℃ of ultrasonic 30min let cool, and add 40% methanol to scale, 0.45 μ m filtering with microporous membrane, get subsequent filtrate 3.9ml and put in the 50ml measuring bottle, add 40% methanol to scale, shake up, and get final product.
Algoscopy: precision is drawn reference substance solution and each 6 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The result: this product content of baicalin is the 80mg/ sheet.
(2) jasminoidin method foundation, chromatographic condition and system suitability are with embodiment 1[assay] (2) lower corresponding contents.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the jasminoidin reference substance, adds 40% methanol and make the solution that concentration is 60 μ g/ml, and get final product.
The preparation of need testing solution: get 1 of this product, grind, accurately weighed, put in the 50ml measuring bottle, add 40% methanol to scale, 25 ℃ of ultrasonic 30min let cool, and add 40% methanol to scale, 0.45 μ m filtering with microporous membrane, get subsequent filtrate 3.9ml and put in the 25ml measuring bottle, add 40% methanol to scale, shake up, and get final product.
Algoscopy: precision is drawn reference substance solution and each 5 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The result: this product Determination of Gardenoside is the 24mg/ sheet.
Embodiment 7
[prescription]
Crude drug and the pharmaceutic adjuvant of above-mentioned weight are made 1000 Chewable Tablets of Chinese traditional medicines altogether.
[method for making] dissolves Radix Scutellariae extract and Fructus Gardeniae extract with an amount of ethanol slight fever; Preparation beta-schardinger dextrin-saturated aqueous solution under 80 ℃ of conditions; Under the stirring condition medicine material alcoholic solution is slowly added in the beta-schardinger dextrin-saturated aqueous solution, constant temperature stirs stopped heating after 1 hour, continues to be stirred to room temperature, get white suspension, cold preservation 96 hours, sucking filtration, precipitate washing with alcohol 3 times, 60 ℃ of drying under reduced pressure are pulverized; With lactose, xylitol, mannitol, soluble starch and sodium carboxymethyl cellulose mix homogeneously, add the medicine material clathrate, mixing, with 20% polyvinylpyrrolidone, 80% alcoholic solution soft material processed, 20 mesh sieves are granulated, 60 ℃ of drying under reduced pressure; Dried granule adds the magnesium stearate mixing with 20 mesh sieve granulate, tabletting, and quality inspection, packing, and get final product.
[discriminating]
(1) get 1 of this product, grind, add 60% methanol 25ml, 25 ℃ of ultrasonic 20min filter, and get subsequent filtrate 1.3ml evaporate to dryness, and residue adds 60% methanol 1ml makes dissolving, as need testing solution.Get the baicalin reference substance an amount of, add 60% methanol and make the solution that concentration is 0.6mg/ml, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 B) test, draw each 4 μ l of above-mentioned need testing solution and reference substance solution, remaining step is differentiated with embodiment 1[] (1) lower corresponding contents.
(2) get 2 of this product, grind, add 60% methanol 25ml, 25 ℃ of ultrasonic 20min filter, and get subsequent filtrate 2.3ml evaporate to dryness, and residue adds 60% methanol 1ml makes dissolving, as need testing solution.Get the jasminoidin reference substance an amount of, add 60% methanol and make the solution that concentration is 3.5mg/ml, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 B) test, draw each 4 μ l of above-mentioned need testing solution and reference substance solution, remaining step is differentiated with embodiment 1[] (2) lower corresponding contents.
[inspection] checks with embodiment 1[] a lower corresponding contents.
[assay]
(1) baicalin method foundation, chromatographic condition and system suitability are with embodiment 1[assay] (1) lower corresponding contents.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the baicalin reference substance, adds 60% methanol and make the solution that concentration is 40 μ g/ml, and get final product.
The preparation of need testing solution: get 1 of this product, grind, accurately weighed, put in the 25ml measuring bottle, add 60% methanol to scale, 25 ℃ of ultrasonic 20min let cool, and add 60% methanol to scale, 0.45 μ m filtering with microporous membrane, get subsequent filtrate 1.4ml and put in the 25ml measuring bottle, add 60% methanol to scale, shake up, and get final product.
Algoscopy: precision is drawn reference substance solution and each 15 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The result: this product content of baicalin is the 80mg/ sheet.
(2) jasminoidin method foundation, chromatographic condition and system suitability are with embodiment 1[assay] (2) lower corresponding contents.
1. the preparation of reference substance solution: it is an amount of that precision takes by weighing the jasminoidin reference substance, adds methanol and make the solution that concentration is 50 μ g/ml, and get final product.
The preparation of need testing solution: get 1 of this product, grind, accurately weighed, put in the 100ml measuring bottle, add methanol to scale, 25 ℃ of ultrasonic 20min let cool, and add methanol to scale, 0.45 μ m filtering with microporous membrane, get subsequent filtrate 4.5ml and put in the 25ml measuring bottle, add methanol to scale, shake up, and get final product.
Algoscopy: precision is drawn reference substance solution and each 6 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The result: this product Determination of Gardenoside is the 24mg/ sheet.
2. the preparation of reference substance solution: it is an amount of that precision takes by weighing the jasminoidin reference substance, adds 60% methanol and make the solution that concentration is 20 μ g/ml, and get final product.
The preparation of need testing solution: get 1 of this product, grind, accurately weighed, put in the 25ml measuring bottle, add 60% methanol to scale, 25 ℃ of ultrasonic 20min let cool, and add 60% methanol to scale, 0.45 μ m filtering with microporous membrane, get subsequent filtrate 1.7ml and put in the 25ml measuring bottle, add 60% methanol to scale, shake up, and get final product.
Algoscopy: precision is drawn reference substance solution and each 15 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The result: this product Determination of Gardenoside is the 24mg/ sheet.
Embodiment 8
[prescription]
Crude drug and the pharmaceutic adjuvant of above-mentioned weight are made 1000 Chewable Tablets of Chinese traditional medicines altogether.
[method for making] dissolves Radix Scutellariae extract and Fructus Gardeniae extract with an amount of ethanol slight fever; Preparation beta-schardinger dextrin-saturated aqueous solution under 80 ℃ of conditions; Under the stirring condition medicine material alcoholic solution is slowly added in the beta-schardinger dextrin-saturated aqueous solution, constant temperature stirs stopped heating after 1.5 hours, continues to be stirred to room temperature, get white suspension, cold preservation 84 hours, sucking filtration, precipitate washing with alcohol 2 times, 50 ℃ of drying under reduced pressure are pulverized; With lactose, xylitol, mannitol, soluble starch and sodium carboxymethyl cellulose mix homogeneously, add the medicine material clathrate, mixing, with 30% polyvinylpyrrolidone, 70% alcoholic solution soft material processed, 30 mesh sieves are granulated, 50 ℃ of drying under reduced pressure; Dried granule adds the magnesium stearate mixing with 30 mesh sieve granulate, tabletting, and quality inspection, packing, and get final product.
[discriminating]
(1) get 1 of this product, grind, add methanol 100ml, 25 ℃ of ultrasonic 20min filter, and get subsequent filtrate 3.8ml evaporate to dryness, and residue adds 40% methanol 1ml makes dissolving, as need testing solution.Get the baicalin reference substance an amount of, add methanol and make the solution that concentration is 2.4mg/ml, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 B) test, draw each 2 μ l of above-mentioned need testing solution and reference substance solution, remaining step is differentiated with embodiment 1[] (1) lower corresponding contents.
(2) get 10 of this product, grind, add methanol 100ml, 25 ℃ of ultrasonic 20min filter, and get subsequent filtrate 3.5ml evaporate to dryness, and residue adds methanol 2ml makes dissolving, as need testing solution.Get the jasminoidin reference substance an amount of, add methanol and make the solution that concentration is 6.5mg/ml, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 B) test, draw each 3 μ l of above-mentioned need testing solution and reference substance solution, remaining step is differentiated with embodiment 1[] (2) lower corresponding contents.
[inspection] checks with embodiment 1[] a lower corresponding contents.
[assay] (1) baicalin method foundation, chromatographic condition and system suitability are with embodiment 1[assay] (1) lower corresponding contents.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the baicalin reference substance, adds methanol and make the solution that concentration is 140 μ g/ml, and get final product.
The preparation of need testing solution: get 2 of this product, grind, accurately weighed, put in the 100ml measuring bottle, add methanol to scale, 25 ℃ of ultrasonic 20min let cool, and add methanol to scale, 0.45 μ m filtering with microporous membrane, get subsequent filtrate 5ml and put in the 50ml measuring bottle, add methanol to scale, shake up, and get final product.
Algoscopy: precision is drawn reference substance solution and each 4 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The result: this product content of baicalin is the 80mg/ sheet.
(2) jasminoidin method foundation, chromatographic condition and system suitability are with embodiment 1[assay] (2) lower corresponding contents.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the jasminoidin reference substance, adds methanol and make the solution that concentration is 50 μ g/ml, and get final product.
The preparation of need testing solution: get 1 of this product, grind, accurately weighed, put in the 100ml measuring bottle, add methanol to scale, 25 ℃ of ultrasonic 20min let cool, and add methanol to scale, 0.45 μ m filtering with microporous membrane, get subsequent filtrate 5ml and put in the 25ml measuring bottle, add methanol to scale, shake up, and get final product.
Algoscopy: precision is drawn reference substance solution and each 6 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The result: this product Determination of Gardenoside is the 24mg/ sheet.
Embodiment 9
[prescription]
Crude drug and the pharmaceutic adjuvant of above-mentioned weight are made 1000 Chewable Tablets of Chinese traditional medicines altogether.
[method for making] dissolves Radix Scutellariae extract and Fructus Gardeniae extract with an amount of ethanol slight fever; Preparation beta-schardinger dextrin-saturated aqueous solution under 80 ℃ of conditions; Under the stirring condition medicine material alcoholic solution is slowly added in the beta-schardinger dextrin-saturated aqueous solution, constant temperature stirs stopped heating after 1.5 hours, continues to be stirred to room temperature, get white suspension, cold preservation 84 hours, sucking filtration, precipitate washing with alcohol 3 times, 50 ℃ of drying under reduced pressure are pulverized; With lactose, xylitol, mannitol, soluble starch and sodium carboxymethyl cellulose mix homogeneously, add the medicine material clathrate, mixing, with 20% polyvinylpyrrolidone, 70% alcoholic solution soft material processed, 30 mesh sieves are granulated, 50 ℃ of drying under reduced pressure; Dried granule adds the magnesium stearate mixing with 30 mesh sieve granulate, tabletting, and quality inspection, packing, and get final product.
[discriminating]
(1) get 1 of this product, grind, get powder 150mg, add 70% methanol 50ml, 25 ℃ of ultrasonic 40min filter, and get subsequent filtrate as need testing solution.Get the baicalin reference substance an amount of, add 70% methanol and make the solution that concentration is 1.2mg/ml, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 B) test, draw each 4 μ l of above-mentioned need testing solution and reference substance solution, remaining step is differentiated with embodiment 1[] (1) lower corresponding contents.
(2) get 3 of this product, grind, add 70% methanol 50ml, 25 ℃ of ultrasonic 40min filter, and get subsequent filtrate 2.4ml evaporate to dryness, and residue adds 70% methanol 1ml makes dissolving, as need testing solution.Get the jasminoidin reference substance an amount of, add 70% methanol and make the solution that concentration is 5.5mg/ml, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 B) test, draw each 4 μ l of above-mentioned need testing solution and reference substance solution, remaining step is differentiated with embodiment 1[] (2) lower corresponding contents.
[inspection] checks with embodiment 1[] a lower corresponding contents.
[assay]
(1) baicalin method foundation, chromatographic condition and system suitability are with embodiment 1[assay] (1) lower corresponding contents.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the baicalin reference substance, adds 70% methanol and make the solution that concentration is 70 μ g/ml, and get final product.
The preparation of need testing solution: get 1 of this product, grind, get powder 150mg, accurately weighed, put in the 50ml measuring bottle, add 70% methanol to scale, 25 ℃ of ultrasonic 40min, let cool, add 70% methanol to scale, 0.45 μ m filtering with microporous membrane, getting subsequent filtrate 2.8ml puts in the 50ml measuring bottle, add 70% methanol to scale, shake up, and get final product.
Algoscopy: precision is drawn reference substance solution and each 9 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The result: this product content of baicalin is the 146.4mg/ sheet.
(2) jasminoidin method foundation, chromatographic condition and system suitability are with embodiment 1[assay] (2) lower corresponding contents.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the jasminoidin reference substance, adds 70% methanol and make the solution that concentration is 40 μ g/ml, and get final product.
The preparation of need testing solution: get 1 of this product, grind, get powder 200mg, accurately weighed, put in the 50ml measuring bottle, add 70% methanol to scale, 25 ℃ of ultrasonic 40min, let cool, add 70% methanol to scale, 0.45 μ m filtering with microporous membrane, getting subsequent filtrate 5.0ml puts in the 50ml measuring bottle, add 70% methanol to scale, shake up, and get final product.
Algoscopy: precision is drawn reference substance solution and each 8 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The result: this product Determination of Gardenoside is the 36mg/ sheet.
Embodiment 10
[prescription]
Crude drug and the pharmaceutic adjuvant of above-mentioned weight are made 1000 Chewable Tablets of Chinese traditional medicines altogether.
[method for making] dissolves Radix Scutellariae extract and Fructus Gardeniae extract with an amount of ethanol slight fever; Preparation beta-schardinger dextrin-saturated aqueous solution under 80 ℃ of conditions; Under the stirring condition medicine material alcoholic solution is slowly added in the beta-schardinger dextrin-saturated aqueous solution, constant temperature stirs stopped heating after 1.5 hours, continues to be stirred to room temperature, get white suspension, cold preservation 84 hours, sucking filtration, precipitate washing with alcohol 3 times, 50 ℃ of drying under reduced pressure are pulverized; With lactose, xylitol, mannitol, soluble starch and sodium carboxymethyl cellulose mix homogeneously, add the medicine material clathrate, mixing, with 20% polyvinylpyrrolidone, 70% alcoholic solution soft material processed, 30 mesh sieves are granulated, 50 ℃ of drying under reduced pressure; Dried granule adds the magnesium stearate mixing with 30 mesh sieve granulate, tabletting, and quality inspection, packing, and get final product.
[discriminating]
(1) get 1 of this product, grind, get powder 260mg, add 70% methanol 50ml, 25 ℃ of ultrasonic 40min filter, and get subsequent filtrate as need testing solution.Get the baicalin reference substance an amount of, add 70% methanol and make the solution that concentration is 1.2mg/ml, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 B) test, draw each 4 μ l of above-mentioned need testing solution and reference substance solution, remaining step is differentiated with embodiment 1[] (1) lower corresponding contents.
(2) get 2 of this product, grind, get powder 450mg, add 70% methanol 50ml, 25 ℃ of ultrasonic 40min filter, and get subsequent filtrate 2.4ml evaporate to dryness, and residue adds 70% methanol 1ml makes dissolving, as need testing solution.Get the jasminoidin reference substance an amount of, add 70% methanol and make the solution that concentration is 5.5mg/ml, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 B) test, draw each 4 μ l of above-mentioned need testing solution and reference substance solution, remaining step is differentiated with embodiment 1[] (2) lower corresponding contents.
[inspection] checks with embodiment 1[] a lower corresponding contents.
[assay]
(1) baicalin method foundation, chromatographic condition and system suitability are with embodiment 1[assay] (1) lower corresponding contents.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the baicalin reference substance, adds 70% methanol and make the solution that concentration is 70 μ g/ml, and get final product.
The preparation of need testing solution: get 1 of this product, grind, get powder 260mg, accurately weighed, put in the 50ml measuring bottle, add 70% methanol to scale, 25 ℃ of ultrasonic 40min, let cool, add 70% methanol to scale, 0.45 μ m filtering with microporous membrane, getting subsequent filtrate 2.8ml puts in the 50ml measuring bottle, add 70% methanol to scale, shake up, and get final product.
Algoscopy: precision is drawn reference substance solution and each 9 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The result: this product content of baicalin is the 84mg/ sheet.
(2) jasminoidin method foundation, chromatographic condition and system suitability are with embodiment 1[assay] (2) lower corresponding contents.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the jasminoidin reference substance, adds 70% methanol and make the solution that concentration is 40 μ g/ml, and get final product.
The preparation of need testing solution: get 1 of this product, grind, get powder 100mg, accurately weighed, put in the 50ml measuring bottle, add 70% methanol to scale, 25 ℃ of ultrasonic 40min, let cool, add 70% methanol to scale, 0.45 μ m filtering with microporous membrane, getting subsequent filtrate 5.0ml puts in the 50ml measuring bottle, add 70% methanol to scale, shake up, and get final product.
Algoscopy: precision is drawn reference substance solution and each 8 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
The result: this product Determination of Gardenoside is the 72mg/ sheet.
Inclusion agents of the present invention is a large class pharmaceutic adjuvant that is applicable to prepare Chewable Tablets of Chinese traditional medicine.In the embodiment that the present invention provides, the inclusion agents that adopts is beta-schardinger dextrin-, but beta-schardinger dextrin-does not limit protection scope of the present invention, and those of ordinary skills can according to practical situation, select suitable inclusion agents.For example, be conducive to the enclose medicine material with the prerequisite of covering its uncomfortable taste under, then can select Hydroxyproply-α-cyclodextrin as inclusion agents.Should be appreciated that equally filler of the present invention, lubricant, correctives, binding agent and disintegrating agent also be not to be limited to the embodiment of the invention, and the claim of only being added limit.
Although foregoing has been done detailed description to the present invention with a general description of the specific embodiments, to those skilled in the art, very likely on basis of the present invention, it is made some modifications or improvement.Therefore, modifications or improvements all belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (8)
1. Chewable Tablets of Chinese traditional medicine for the treatment of upper respiratory tract infection, it is characterized in that: described Chewable Tablets of Chinese traditional medicine is made by crude drug and the pharmaceutic adjuvant of following percentage by weight:
The main effective ingredient of described Radix Scutellariae extract is baicalin; The weight percent content of baicalin is for being not less than 70% in its described Radix Scutellariae extract;
The main effective ingredient of described Fructus Gardeniae extract is jasminoidin; The weight percent content of jasminoidin is for being not less than 50% in its described Fructus Gardeniae extract.
2. Chewable Tablets of Chinese traditional medicine according to claim 1, it is characterized in that: described inclusion agents is selected from one or more in alpha-cyclodextrin, beta-schardinger dextrin-, gamma-cyclodextrin, Hydroxyproply-α-cyclodextrin, HP-β-CD, hydroxypropyl-gamma-cyclodextrin, methyl-beta-schardinger dextrin-, carboxymethyl-beta-cyclodextrin or one chlorotriazine-beta-schardinger dextrin-; Described filler is selected from one or more in lactose, sorbitol, mannitol, xylitol, microcrystalline Cellulose, dextrin, sucrose, fructose, glucose, soluble starch or the Mel; Described lubricant is selected from one or more in magnesium stearate, micropowder silica gel, Pulvis Talci, Polyethylene Glycol or the microcrystalline Cellulose; Described correctives is selected from that sucrose, A Siba are sweet, in stevioside, acesulfame potassium, cyclamate, glycyrrhizin, chocolate, organic acid, acylate or the essence one or more; Described binding agent is selected from the pressed powder of the pressed powder of gelatin, Resina persicae, tragcanth, xanthan gum, propolis, carrageenan, guar gum, agar, arabic gum, sodium alginate, pectin, Semen Lini glue, the polysaccharide that condenses, pulullan, gellan gum, propylene glycol alginate, locust bean gum or solution, Konjac glucomannan or in solution, ethanol, polyglycol solution, polyvinylpyrrolidonesolution solution or the cellulose derivative alcoholic solution one or more; Described disintegrating agent is selected from one or more in sodium carboxymethyl cellulose, crospolyvinylpyrrolidone, low-substituted hydroxypropyl cellulose, Sodium Hydroxymethyl Stalcs, cross-linking sodium carboxymethyl cellulose, hydroxypropyl starch or the micropowder silica gel.
3. Chewable Tablets of Chinese traditional medicine according to claim 1 is characterized in that: the percentage by weight of preferred crude drug and pharmaceutic adjuvant is:
The main effective ingredient of described Radix Scutellariae extract is baicalin; The weight percent content of baicalin is for being not less than 70% in its described Radix Scutellariae extract;
The main effective ingredient of described Fructus Gardeniae extract is jasminoidin; The weight percent content of jasminoidin is for being not less than 50% in its described Fructus Gardeniae extract.
4. described Chewable Tablets of Chinese traditional medicine one of according to claim 1-3, it is characterized in that: the sheet of described Chewable Tablets of Chinese traditional medicine heavily is 100～1000 mg.
5. the preparation method such as one of claim 1-3 described Chewable Tablets of Chinese traditional medicine is characterized in that, may further comprise the steps: Radix Scutellariae extract and Fructus Gardeniae extract are dissolved with the ethanol slight fever; Under 80 ℃ of conditions the inclusion agents water is made saturated solution; Under the stirring condition medicine material alcoholic solution slowly is added in the inclusion agents saturated solution, stopped heating behind constant temperature stirring 1～2 h, continue to be stirred to room temperature, get white suspension, cold preservation 72～120 h, sucking filtration, precipitate washing with alcohol 2～4 times, 40～60 ℃ of drying under reduced pressure are pulverized, and obtain the medicine material clathrate; With filler, correctives and disintegrating agent mix homogeneously, add the medicine material clathrate, mixing, with 15%～30% binding agent, 60%～80% alcoholic solution soft material processed, 20～40 mesh sieves are granulated, 40～60 ℃ of dryings; Dried granule adds the lubricant mixing with 20～40 mesh sieve granulate, tabletting, and quality inspection, packing namely gets Chewable Tablets of Chinese traditional medicine.
6. the preparation method of Chewable Tablets of Chinese traditional medicine according to claim 5, it is characterized in that, the preparation method of described Radix Scutellariae extract may further comprise the steps: get Radix Scutellariae and smash, add in 10 times of amount boiling water, decoct 3 times, 2 h/ time, collecting decoction, centrifugal, the centrifugal liquid concentrating under reduced pressure becomes every 1ml to contain the medicinal liquid (the room temperature relative density is about 1.15) of 0.25g crude drug, uses 2mol.L
-1Hydrochloric acid solution is transferred pH to 2, and 80 ℃ of insulation 60min leave standstill 12h, and collecting precipitation and being suspended in waits in the water gaging, transfers pH to 7 with 40% sodium hydroxide solution, adds ethanol, make to contain the alcohol amount and reach 50%, and fully stirring, filtration, filtrate is used 2mol.L
-1Hydrochloric acid solution is transferred pH to 2, and 80 ℃ of insulation 60min leave standstill 12h, and it is 4.0 that collecting precipitation also is washed till pH with 50% ethanol, and drying under reduced pressure namely gets Radix Scutellariae extract.
7. the preparation method of Chewable Tablets of Chinese traditional medicine according to claim 5, it is characterized in that, the preparation method of described Fructus Gardeniae extract may further comprise the steps: get Fructus Gardeniae and smash, add 8 times of amounts of 70% ethanol, atmospheric pressure reflux 2 times, each 1.5 h, merge extractive liquid,, centrifugal, the centrifugal liquid Recycled ethanol, concentrating under reduced pressure, water is made the medicinal liquid (the room temperature relative density is about 1.12) that every 1ml contains the 0.5g crude drug, and is centrifugal, and centrifugal liquid is adsorbed with the HPD450 macroporous adsorbent resin bed that is equivalent to 2 times of crude drug amounts, flow velocity is 0.5BV/h, adsorb the complete rear 4BV of using 70% ethanol elution, flow velocity 2BV/h, eluent filters, Recycled ethanol, concentrating under reduced pressure, drying namely gets Fructus Gardeniae extract.
8. the quality determining method such as one of claim 1-7 described Chewable Tablets of Chinese traditional medicine is characterized in that, may further comprise the steps:
(1) differentiates
A, get 1～4 of this product, grind, add 30～100% methanol, 20～100ml, 25 ℃ of ultrasonic 20～40min filter, and subsequent filtrate is as need testing solution, or get subsequent filtrate 1～5ml evaporate to dryness, and residue adds methanol 1～2ml makes dissolving, as need testing solution; Get the baicalin reference substance an amount of, add 30～100% methanol and make the solution that concentration is 0.5～3mg/ml, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2010 B thin layer chromatography, draw each 2～10 μ l of above-mentioned need testing solution and reference substance solution, put respectively in same take the carboxymethylcellulose sodium solution that contains 4% sodium acetate on the silica gel g thin-layer plate of binding agent, take ethyl acetate-butanone of volume ratio 5:3:1:1-formic acid-water as developing solvent, pre-equilibration 30min launches, and takes out, dry, spray is with 1% ferric chloride alcoholic solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, aobvious one identical dirty-green speckle;
B, get 1～10 of this product, grind, add 30～100% methanol, 20～100ml, 25 ℃ of ultrasonic 20～40min filter, and subsequent filtrate is as need testing solution, or get subsequent filtrate 1～5ml evaporate to dryness, and residue adds methanol 1～2ml makes dissolving, as need testing solution; Get the jasminoidin reference substance an amount of, add 30～100% methanol and make the solution that concentration is 2～10mg/ml, in contrast product solution.Test according to an appendix VI of Chinese Pharmacopoeia version in 2010 B thin layer chromatography, draw each 2～10 μ l of above-mentioned need testing solution and reference substance solution, put respectively in same take the carboxymethylcellulose sodium solution that contains 4% sodium acetate on the silica gel g thin-layer plate of binding agent, ethyl acetate-acetone take volume ratio as 5:5:1:1-formic acid-water is developing solvent, launch, take out, dry, spray is heated to the speckle colour developing at 110 ℃ clear with sulphuric acid ethanol (5 → 10) solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, the speckle of aobvious same color;
(2) check
This product should meet the every regulation under an appendix I of Chinese Pharmacopoeia version in 2010 the D rules of preparations tablet item;
(3) assay
According to an appendix VI of Chinese Pharmacopoeia version in 2010 D high effective liquid chromatography for measuring;
A, baicalin
Chromatographic condition and system suitability: be filler with octadecylsilane chemically bonded silica, 30 ℃ of column temperatures, take the methanol-water-phosphoric acid of volume ratio 47:53:0.2 as mobile phase, flow velocity is 1ml/min, the detection wavelength is 280nm, and theoretical cam curve is calculated by the baicalin peak should be not less than 2500;
The preparation of reference substance solution: it is an amount of that precision takes by weighing the baicalin reference substance, adds 30～100% methanol and make the solution that concentration is 30～150 μ g/ml, and get final product;
The preparation of need testing solution: get 1～4 of this product, grind, accurately weighed, put in 10～100ml measuring bottle, add 30～100% methanol to scale, 25 ℃ of ultrasonic 20～40min let cool, add 30～100% methanol to scale, 0.45 μ m filtering with microporous membrane is got subsequent filtrate 1～5ml and is put in 5～50ml measuring bottle, adds 30～100% methanol to scale, shake up, and get final product;
Algoscopy: precision is drawn reference substance solution and each 2～15 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product;
B, jasminoidin
Chromatographic condition and system suitability: be filler with octadecylsilane chemically bonded silica, 30 ℃ of column temperatures, the acetonitrile-water take volume ratio as 15:85 is mobile phase, flow velocity is 1ml/min, the detection wavelength is 238nm, and theoretical cam curve is calculated by the jasminoidin peak should be not less than 1500;
The preparation of reference substance solution: it is an amount of that precision takes by weighing the jasminoidin reference substance, adds 30～100% methanol and make the solution that concentration is 10～100 μ g/ml, and get final product;
The preparation of need testing solution: get 1～10 of this product, grind, accurately weighed, put in 10～100ml measuring bottle, add 30～100% methanol to scale, 25 ℃ of ultrasonic 30min let cool, add 30～100% methanol to scale, 0.45 μ m filtering with microporous membrane is got subsequent filtrate 1～5ml and is put in 5～50ml measuring bottle, adds 30～100% methanol to scale, shake up, and get final product;
Algoscopy: precision is drawn reference substance solution and each 2～15 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103285121A (en) * | 2013-06-26 | 2013-09-11 | 重庆邮电大学 | Chinese medicine soft capsule for treating upper respiratory infection and preparation method as well as quality detection method thereof |
| CN103630648A (en) * | 2013-10-15 | 2014-03-12 | 滨州医学院附属医院 | Method for detecting anti-infective drug |
| CN105166715A (en) * | 2015-10-20 | 2015-12-23 | 山东颐养天年营养食品科技发展有限公司 | Compound wheat sprout chewable tablets and preparation method thereof |
| CN105548452A (en) * | 2016-02-05 | 2016-05-04 | 四川德成动物保健品有限公司 | Thin-layer chromatography detection method of cape jasmines in heat-clearing and detoxifying powder |
| CN105616921A (en) * | 2016-01-20 | 2016-06-01 | 张俊志 | Traditional Chinese medicine composition for treating upper respiratory tract infection and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1541652A (en) * | 2003-11-05 | 2004-11-03 | 江苏扬子江药业集团有限公司 | Traditional Chinese medicine for treating upper respiratory tract infection and its preparation method |
| CN1730052A (en) * | 2005-04-11 | 2006-02-08 | 成都精晶天然药物开发有限公司 | Cape jasmine and baikal skullcap root di-glycocide injection and its preparation process and purposes |
| CN1730051A (en) * | 2005-04-11 | 2006-02-08 | 成都百康医药工业药理毒理研究院 | Injection for treating acute cholecystitis and method for preparing the same |
| CN1748741A (en) * | 2005-10-20 | 2006-03-22 | 北京阜康仁生物制药科技有限公司 | Little leaf deervetch herb acne removing preparation and new preparing method |
| US20110183015A1 (en) * | 2010-01-22 | 2011-07-28 | Chen-Yu Lee | Medical composition for inhibiting the growth of cancer stem cell |
| WO2012050396A2 (en) * | 2010-10-14 | 2012-04-19 | 주식회사 한국전통의학연구소 | Pharmaceutical composition including herbal medicine extract for preventing or treating liver cancer |
-
2012
- 2012-12-12 CN CN2012105334635A patent/CN102940708A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1541652A (en) * | 2003-11-05 | 2004-11-03 | 江苏扬子江药业集团有限公司 | Traditional Chinese medicine for treating upper respiratory tract infection and its preparation method |
| CN1730052A (en) * | 2005-04-11 | 2006-02-08 | 成都精晶天然药物开发有限公司 | Cape jasmine and baikal skullcap root di-glycocide injection and its preparation process and purposes |
| CN1730051A (en) * | 2005-04-11 | 2006-02-08 | 成都百康医药工业药理毒理研究院 | Injection for treating acute cholecystitis and method for preparing the same |
| CN1748741A (en) * | 2005-10-20 | 2006-03-22 | 北京阜康仁生物制药科技有限公司 | Little leaf deervetch herb acne removing preparation and new preparing method |
| US20110183015A1 (en) * | 2010-01-22 | 2011-07-28 | Chen-Yu Lee | Medical composition for inhibiting the growth of cancer stem cell |
| WO2012050396A2 (en) * | 2010-10-14 | 2012-04-19 | 주식회사 한국전통의학연구소 | Pharmaceutical composition including herbal medicine extract for preventing or treating liver cancer |
Non-Patent Citations (1)
| Title |
|---|
| 季申等: "茵栀黄注射液质量标准研究", 《中成药》, vol. 31, no. 12, 31 December 2009 (2009-12-31) * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103285121A (en) * | 2013-06-26 | 2013-09-11 | 重庆邮电大学 | Chinese medicine soft capsule for treating upper respiratory infection and preparation method as well as quality detection method thereof |
| CN103630648A (en) * | 2013-10-15 | 2014-03-12 | 滨州医学院附属医院 | Method for detecting anti-infective drug |
| CN105166715A (en) * | 2015-10-20 | 2015-12-23 | 山东颐养天年营养食品科技发展有限公司 | Compound wheat sprout chewable tablets and preparation method thereof |
| CN105616921A (en) * | 2016-01-20 | 2016-06-01 | 张俊志 | Traditional Chinese medicine composition for treating upper respiratory tract infection and preparation method thereof |
| CN105548452A (en) * | 2016-02-05 | 2016-05-04 | 四川德成动物保健品有限公司 | Thin-layer chromatography detection method of cape jasmines in heat-clearing and detoxifying powder |
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Application publication date: 20130227 |