CN104606226B - Anti-inflammation Chinese medicine suppository and preparation method thereof and quality control method - Google Patents
Anti-inflammation Chinese medicine suppository and preparation method thereof and quality control method Download PDFInfo
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Abstract
The present invention relates to a kind of anti-inflammation Chinese medicine suppository and preparation method thereof and quality control method, belong to technical field of traditional Chinese medicines.The anti-inflammation Chinese medicine suppository includes following component in parts by weight：48 52 parts of alum, 8 12 parts of fibrauretine, 38 42 parts of red halloysite, 8 12 parts of borneol, 18 22 parts of polyoxyethylene sorbitan monoleate, glycerin gelatine are 900 920 parts.Preparation method of the present invention is simple, obtained excellent product performance, there is antibacterial, anti-inflammatory, detumescence, analgesic, hemostasis, convergence and removing necrosis, promoting granulation, effect highly significant, it can be widely used for the preventing and treating of anal intestine, the inflammatory disease of gynaecology, and the control for passing through method of quality control so that ensured the effect of product.
Description
Technical field
The invention belongs to technical field of traditional Chinese medicines, and in particular to a kind of anti-inflammation Chinese medicine suppository and preparation method thereof and Quality Control
Method.
Background technology
As all kinds of antibiotic using penicillin as representative continuously emerge, bacterial infection disease is effectively controlled, from
And antibiotic is set to turn into the powerful mean that the mankind resist pathogenic bacterial infection.But in recent years, antibiotic is widely used in people for a long time
Causing the drug resistance of bacterium constantly to strengthen, Resistant frequency gradually increases, so that conventional antibiotic can not meet clinical needs.With
Global disease spectrum and the important change of medical model, China progressively integrates with World Economics, culture and drug level, compatriots
The understanding of antibiotic is enhanced, it is appreciated that many adverse reactions that antibiotic is brought and its corresponding drug resistance
Influence, people are filled with expectation to Chinese medicine maintaining healthy and disease preventing and treating.Medical field is also expected that by the rational use of medicines and exploitation
Medicine new drug come tackle constantly caused by drug-fast bacteria.The present inventor is based on this and opened with modern Chinese herbal medicine extractive technique and preparation technique
Definite, the with strong points Chinese medicine of antibacterial effect is sent out, the needs of clinical treatment are met with this.
Hemorrhoid are common frdquently encountered disease, and the more common disease of cervicitis, vaginitis of anal intestine and gynaecology is all most currently on the market
Hormone medicine is all used, and the toxic side effect of these medicines is big.Therefore how overcome the deficiencies in the prior art be at present in
The problem of medicine technical field urgent need to resolve.
The content of the invention
The invention aims to solve the deficiencies in the prior art, there is provided a kind of anti-inflammation Chinese medicine suppository and its preparation
Method and quality control method, the preparation method is simple, obtained excellent product performance, and by the control of method of quality control, makes
The effect of obtaining product is ensured.
The technical solution adopted by the present invention is as follows：
A kind of anti-inflammation Chinese medicine suppository, including following component in parts by weight：
Alum 48-52 parts, fibrauretine 8-12 parts, red halloysite 38-42 parts, borneol 8-12 parts, polyoxyethylene sorbitan monoleate 18-22 parts,
Glycerin gelatine is 900-920 parts.
It is further preferred that described anti-inflammation Chinese medicine suppository, including following component in parts by weight：
50 parts of alum, 10 parts of fibrauretine, 40 parts of red halloysite, 10 parts of borneol, 20 parts of polyoxyethylene sorbitan monoleate, glycerin gelatine 900-
920 parts.
The present invention also provides a kind of preparation method of anti-inflammation Chinese medicine suppository, comprises the following steps：
Step (1), alum, red halloysite and borneol are respectively crushed into fine powder；
Step (2), fibrauretine is crossed 100 mesh sieves；
Step (3), take red halloysite fine powder to add water for injection 390-410 parts, adjust pH to 3.0 with watery hydrochloric acid, heating is boiled
Boiling, boil 1 hour, then stop heating, after being cooled to room temperature, standing makes insoluble matter fully precipitate, and takes supernatant and filters, obtains
To clear filtrate；
Step (4), the clear filtrate that step (3) obtains is heated to boiling, then adds alum fine powder, stirring makes completely molten
Solution, filters, filtrate is then concentrated into 49-51 parts, be cooled to 50-60 DEG C, and maintain the temperature at 50-60 DEG C while hot；
Glycerin gelatine, is heated to 50-60 DEG C by step (5), is made to be completely dissolved, is then slowly added into step while stirring
(4) solution obtained by, fibrauretine, borneol fine powder and the polyoxyethylene sorbitan monoleate for having crossed 100 mesh sieves, stir to well mixed, reverse mould system
Grain, cool down, packaging, that is, obtain anti-inflammation Chinese medicine suppository.
It is further preferred that the time of repose described in step (3) is 24 hours.
The method of quality control of anti-inflammation Chinese medicine suppository, comprises the following steps made from above-mentioned preparation method：
First, character detection：Anti-inflammation Chinese medicine suppository is the bolt of yellow；
Second, differentiate：
The preparation of need testing solution：Anti-inflammation Chinese medicine suppository is taken, is put in evaporating dish, is heated to melting in water-bath, not
Disconnected stirring, makes to be well mixed, and cools down, and precision weighs 10g, put in 100ml measuring bottles, adds methanol 80-85ml, puts in 50 DEG C of water-baths and adds
Heat, after constantly shaking makes dissolving, then shake 5 minutes, let cool, with methanol dilution to scale, shake up, filter, discard coarse filtration liquid, essence
It is close to measure subsequent filtrate 10ml, put in 100ml measuring bottles, be 70% methanol dilution to scale with volume fraction, shake up, filter membrane filtration,
Produce need testing solution；
A. the detection of alum
Take need testing solution 2ml, to gelatinous precipitate is generated western plain sodium sulfonate test solution is added dropwise few drops in ammonification test solution, and precipitation is aobvious
Cherry red；
B. the thin-layer chromatography detection of the palmatin hydrochloride in fibrauretine
Take need testing solution；Palmatin hydrochloride reference substance separately is taken, adds ethanol that solution of every 1ml containing 0.1mg is made, as right
According to product solution；According to thin-layered chromatography (《Chinese Pharmacopoeia》One B of annex VI of version in 2010) experiment, it is molten that above-mentioned test sample is drawn respectively
Liquid and each 5ul of reference substance solution, put respectively on same silica gel g thin-layer plate, using volume ratio as 7:1:2 isoamyl acetate-nothing
The mixed solvent of water-ethanol-formic acid is solvent, is deployed, and takes out, dries, put under uviol lamp, inspected in 365um, test sample color
In spectrum on position corresponding with reference substance chromatogram, show the fluorescence spot of identical color；
C. the detection of borneol
Take need testing solution 1ml, 1% vanillin-sulfuric acid solution 3-5 drops of dropwise addition, i.e., aobvious purple；
3rd, content detection：
(1), fibrauretine assay
According to high performance liquid chromatography (《Chinese Pharmacopoeia》Attached VI D of version one in 2010) measure；
Chromatographic condition and system suitability：It is filler with octadecylsilane chemically bonded silica；Using volume ratio as 30:70:
The mixed solvent of 0.2 acetonitrile-water-phosphoric acid is mobile phase；Flow velocity is 1.0ml/min, and column temperature is that 30 DEG C of Detection wavelengths are
272nm, number of theoretical plate is calculated by palmatin hydrochloride peak should be not less than 1800；
The preparation of reference substance solution：Palmatin hydrochloride reference substance is taken, adds 70% methanol that solution of every 1ml containing 70ug is made,
Produce；
The preparation of need testing solution：Anti-inflammation Chinese medicine suppository is taken, is put in evaporating dish, is heated to melting in water-bath, not
Disconnected stirring, makes to be well mixed, and cools down, and precision weighs 10g, put in 100ml measuring bottles, adds methanol 80-85ml, puts in 50 DEG C of water-baths and adds
Heat, after constantly shaking makes dissolving, then shake 5 minutes, let cool, with methanol dilution to scale, shake up, filter, discard coarse filtration liquid, essence
It is close to measure subsequent filtrate 10ml, put in 100ml measuring bottles, be 70% methanol dilution to scale with volume fraction, shake up, filter membrane filtration,
Produce need testing solution；
Determination method：It is accurate respectively to draw reference substance solution and each 10ul of need testing solution, liquid chromatograph is injected separately into, is surveyed
It is fixed, produce；
Anti-inflammation Chinese medicine suppository is containing fibrauretine with palmatin hydrochloride (C21H21NO4HCl) calculate, should be labelled amount
70-115%；
(2) alum assay
The preparation of need testing solution：Anti-inflammation Chinese medicine suppository is taken, is shredded, is mixed, precision weighs 50g, puts 50ml measuring bottles
In, add water about to 40ml, to put in 60-65 DEG C of water-bath, shaking makes dissolving, then takes out and lets cool, be diluted with water to scale, shakes up,
Filtration, discards coarse filtration liquid, subsequent filtrate is put in measuring bottle, produce；
Precision draws need testing solution 20ml, adds acetic acid-ammonium acetate buffer 20ml that pH is 6.0, then add 0.05mol/L
The acetic acid disodium titrating solution 25ml of two ammonium of second four, heating boils, boils 8-10 minutes, let cool, and adds xylenol orange indicator solution 1ml,
Solution is titrated to 0.05mol/L zinc titrating solution and is changed into red from yellow, and the result of titration is corrected with blank test；
Per 1ml 0.05mol/L aqueous sulfuric acid aluminium potassium [KAl (SO of the acetic acid disodium titrating solution of two ammonium of second four equivalent to 23.72mg4)2·
12H2O]；
Anti-inflammation Chinese medicine suppository is containing alum with aqueous sulfuric acid aluminium potassium [KAl (SO4)2.12H2O] calculate, it should be labelled amount
80%-120%.
It is other：Should meet relevant every regulation under suppository item (《Chinese Pharmacopoeia》One W of annex I of version in 2010).
Note：The conventional proportioning of glycerin gelatine is water:Gelatin:Glycerine=10:20:70, but adjustment proportioning can be required according to different.
Compared with prior art, its advantage is the present invention：
The problems such as present invention solution patient can not voluntarily use and application cost is high, makes application expand from local injection
To ear nose, the preventing and treating of inflammatory disease etc. in oral cavity, anal intestine, surgery, gynaecology, burn and scald, topical route is changed into；The present invention considers
The problem of can medicament mucosa, hypodermis absorb, and successfully solve this problem, product is haveed the function that sustained release,
Considerably increase efficacy time.
Product of the present invention has the function that antibacterial, anti-inflammatory, detumescence, analgesic, hemostasis, convergence and removing necrosis, promoting granulation, and effect is very
Significantly.For dressing, it can reach and be not required to the purpose of the antibacterial-anti-inflammatory drug with Formulations for systemic administration again (suppository is local administration, such as logical
It is exactly Formulations for systemic administration to cross oral or injection), and it is easy to carry, use freely, application easy to spread.
Product preparation method of the present invention is simple, obtained excellent product performance, and by the control of method of quality control, makes
The effect of obtaining product is ensured.
Embodiment
With reference to embodiment, the present invention is described in further detail.
It will be understood to those of skill in the art that the following example is merely to illustrate the present invention, and it should not be regarded as limiting this hair
Bright scope.In the examples where no specific technique or condition is specified, according to the technology or condition described by document in the art
Or carried out according to product description.Agents useful for same or the unreceipted production firm person of instrument, it is that can be obtained by buying
Conventional products.
Embodiment 1
A kind of anti-inflammation Chinese medicine suppository, including following component in parts by weight：
Alum 48g, fibrauretine 8g, red halloysite 38g, borneol 8g, polyoxyethylene sorbitan monoleate 18g, glycerin gelatine 900g.
The preparation method of the anti-inflammation Chinese medicine suppository of the present embodiment, comprises the following steps：
Step (1), alum, red halloysite and borneol are respectively crushed into fine powder；
Step (2), fibrauretine is crossed 100 mesh sieves；
Step (3), take red halloysite fine powder to add water for injection 390ml, adjust pH to 3.0 with watery hydrochloric acid, heating is boiled, and is boiled
Boiling 1 hour, then stop heating, after being cooled to room temperature, standing 24 hours makes insoluble matter fully precipitate, and takes supernatant and filters,
Obtain clear filtrate；
Step (4), the clear filtrate that step (3) obtains is heated to boiling, then adds alum fine powder, stirring makes completely molten
Solution, filters, filtrate is then concentrated into 49ml, be cooled to 50 DEG C, and maintain the temperature at 50 DEG C while hot；
Glycerin gelatine, is heated to 50 DEG C, makes to be completely dissolved by step (5), is then slowly added into step (4) institute while stirring
Solution, crossed fibrauretine, borneol fine powder and the polyoxyethylene sorbitan monoleate of 100 mesh sieves, stir to well mixed, reverse mould granulation 500
Grain, cool down, packaging, that is, obtain anti-inflammation Chinese medicine suppository.
Embodiment 2
A kind of anti-inflammation Chinese medicine suppository, including following component in parts by weight：
Alum 52g, fibrauretine 12g, red halloysite 42g, borneol 12g, polyoxyethylene sorbitan monoleate 22g, glycerin gelatine 920g.
The preparation method of the anti-inflammation Chinese medicine suppository of the present embodiment, comprises the following steps：
Step (1), alum, red halloysite and borneol are respectively crushed into fine powder；
Step (2), fibrauretine is crossed 100 mesh sieves；
Step (3), take red halloysite fine powder to add water for injection 400ml, adjust pH to 3.0 with watery hydrochloric acid, heating is boiled, and is boiled
Boiling 1 hour, then stop heating, after being cooled to room temperature, standing 24 hours makes insoluble matter fully precipitate, and takes supernatant and filters,
Obtain clear filtrate；
Step (4), the clear filtrate that step (3) obtains is heated to boiling, then adds alum fine powder, stirring makes completely molten
Solution, filters, filtrate is then concentrated into 50ml, be cooled to 56 DEG C, and maintain the temperature at 56 DEG C while hot；
Glycerin gelatine, is heated to 56 DEG C, makes to be completely dissolved by step (5), is then slowly added into step (4) institute while stirring
Solution, crossed fibrauretine, borneol fine powder and the polyoxyethylene sorbitan monoleate of 100 mesh sieves, stir to well mixed, reverse mould granulation 500
Grain, cool down, packaging, that is, obtain anti-inflammation Chinese medicine suppository.
Embodiment 3
A kind of anti-inflammation Chinese medicine suppository, including following component in parts by weight：
Alum 50g, fibrauretine 10g, red halloysite 40g, borneol 10g, polyoxyethylene sorbitan monoleate 20g, glycerin gelatine 910g.
The preparation method of the anti-inflammation Chinese medicine suppository of the present embodiment, comprises the following steps：
Step (1), alum, red halloysite and borneol are respectively crushed into fine powder；
Step (2), fibrauretine is crossed 100 mesh sieves；
Step (3), take red halloysite fine powder to add water for injection 410ml, adjust pH to 3.0 with watery hydrochloric acid, heating is boiled, and is boiled
Boiling 1 hour, then stop heating, after being cooled to room temperature, standing 24 hours makes insoluble matter fully precipitate, and takes supernatant and filters,
Obtain clear filtrate；
Step (4), the clear filtrate that step (3) obtains is heated to boiling, then adds alum fine powder, stirring makes completely molten
Solution, filters, filtrate is then concentrated into 51ml, be cooled to 60 DEG C, and maintain the temperature at 60 DEG C while hot；
Glycerin gelatine, is heated to 60 DEG C, makes to be completely dissolved by step (5), is then slowly added into step (4) institute while stirring
Solution, crossed fibrauretine, borneol fine powder and the polyoxyethylene sorbitan monoleate of 100 mesh sieves, stir to well mixed, reverse mould granulation 500
Grain, cool down, packaging, that is, obtain anti-inflammation Chinese medicine suppository.
Embodiment 4
A kind of anti-inflammation Chinese medicine suppository, including following component in parts by weight：
Alum 50g, fibrauretine 10g, red halloysite 40g, borneol 10g, polyoxyethylene sorbitan monoleate 20g, glycerin gelatine 900g.
The preparation method of the anti-inflammation Chinese medicine suppository of the present embodiment is same as Example 2.It is made 500.
Embodiment 5
A kind of anti-inflammation Chinese medicine suppository, including following component in parts by weight：
Alum 50g, fibrauretine 10g, red halloysite 40g, borneol 10g, polyoxyethylene sorbitan monoleate 20g, glycerin gelatine 920g.
The preparation method of the anti-inflammation Chinese medicine suppository of the present embodiment is same as Example 2.It is made 500.
The method of quality control of product obtained by embodiment 1-5, comprises the following steps：
First, character detection：Anti-inflammation Chinese medicine suppository is the bolt of yellow；
Second, differentiate：
The preparation of need testing solution：Anti-inflammation Chinese medicine suppository is taken, is put in evaporating dish, is heated to melting in water-bath, not
Disconnected stirring, makes to be well mixed, and cools down, and precision weighs 10g, put in 100ml measuring bottles, adds methanol 80-85ml, puts in 50 DEG C of water-baths and adds
Heat, after constantly shaking makes dissolving, then shake 5 minutes, let cool, with methanol dilution to scale, shake up, filter, discard coarse filtration liquid, essence
It is close to measure subsequent filtrate 10ml, put in 100ml measuring bottles, be 70% methanol dilution to scale with volume fraction, shake up, filter membrane filtration,
Produce need testing solution；
A. the detection of alum
Take need testing solution 2ml, to gelatinous precipitate is generated western plain sodium sulfonate test solution is added dropwise few drops in ammonification test solution, and precipitation is aobvious
Cherry red；
B. the thin-layer chromatography detection of the palmatin hydrochloride in fibrauretine
Take need testing solution；Palmatin hydrochloride reference substance separately is taken, adds ethanol that solution of every 1ml containing 0.1mg is made, as right
According to product solution；According to thin-layered chromatography (《Chinese Pharmacopoeia》One B of annex VI of version in 2010) experiment, it is molten that above-mentioned test sample is drawn respectively
Liquid and each 5ul of reference substance solution, put respectively on same silica gel g thin-layer plate, using volume ratio as 7:1:2 isoamyl acetate-nothing
The mixed solvent of water-ethanol-formic acid is solvent, is deployed, and takes out, dries, put under uviol lamp, inspected in 365um, test sample color
In spectrum on position corresponding with reference substance chromatogram, show the fluorescence spot of identical color；
C. the detection of borneol
Take need testing solution 1ml, 1% vanillin-sulfuric acid solution 3-5 drops of dropwise addition, i.e., aobvious purple；
3rd, content detection：
(1), fibrauretine assay
According to high performance liquid chromatography (《Chinese Pharmacopoeia》Attached VI D of version one in 2010) measure；
Chromatographic condition and system suitability：It is filler with octadecylsilane chemically bonded silica；Using volume ratio as 30:70:
The mixed solvent of 0.2 acetonitrile-water-phosphoric acid is mobile phase；Flow velocity is 1.0ml/min, and column temperature is that 30 DEG C of Detection wavelengths are
272nm, number of theoretical plate is calculated by palmatin hydrochloride peak should be not less than 1800；
The preparation of reference substance solution：Palmatin hydrochloride reference substance is taken, adds 70% methanol that solution of every 1ml containing 70ug is made,
Produce；
The preparation of need testing solution：Anti-inflammation Chinese medicine suppository is taken, is put in evaporating dish, is heated to melting in water-bath, not
Disconnected stirring, makes to be well mixed, and cools down, and precision weighs 10g, put in 100ml measuring bottles, adds methanol 80-85ml, puts in 50 DEG C of water-baths and adds
Heat, after constantly shaking makes dissolving, then shake 5 minutes, let cool, with methanol dilution to scale, shake up, filter, discard coarse filtration liquid, essence
It is close to measure subsequent filtrate 10ml, put in 100ml measuring bottles, be 70% methanol dilution to scale with volume fraction, shake up, filter membrane filtration,
Produce need testing solution；
Determination method：It is accurate respectively to draw reference substance solution and each 10ul of need testing solution, liquid chromatograph is injected separately into, is surveyed
It is fixed, produce；
Anti-inflammation Chinese medicine suppository is containing fibrauretine with palmatin hydrochloride (C21H21NO4HCl) calculate, should be labelled amount
70-115%；
(2) alum assay
The preparation of need testing solution：Anti-inflammation Chinese medicine suppository is taken, is shredded, is mixed, precision weighs 5g, puts 50ml measuring bottles
In, 40ml is added water to, is put in 60-65 DEG C of water-bath, shaking makes dissolving, then takes out and lets cool, be diluted with water to scale, shakes up, and filters
Cross, discard coarse filtration liquid, subsequent filtrate is put in measuring bottle, produce；
Precision draws need testing solution 20ml, adds acetic acid-ammonium acetate buffer 20ml that pH is 6.0, then add 0.05mol/L
The acetic acid disodium titrating solution 25ml of two ammonium of second four, heating boils, boils 8-10 minutes, let cool, and adds xylenol orange indicator solution 1ml,
Solution is titrated to 0.05mol/L zinc titrating solution and is changed into red from yellow, and the result of titration is corrected with blank test；
Per 1ml 0.05mol/L aqueous sulfuric acid aluminium potassium [KAl (SO of the acetic acid disodium titrating solution of two ammonium of second four equivalent to 23.72mg4)2·
12H2O]；
Anti-inflammation Chinese medicine suppository is containing alum with aqueous sulfuric acid aluminium potassium [KAl (SO4)2.12H2O] calculate, it is labelled amount
80%-120%.
It is other：Should meet relevant every regulation under suppository item (《Chinese Pharmacopoeia》One W of annex I of version in 2010).
Detected through the above method, it is found that the product of embodiment 1- embodiments 5 meets the quality standard.
Pharmacodynamics test
A, anti-inflammation Chinese medicine suppository vitro antibacterial activity (cylinder-plate method)
Experiment material
1st, medicine：Anti-inflammation Chinese medicine suppository of the present invention, lot number 20140101.Injection benzyl penicillin, Kunming pharmacy share
Co., Ltd's product, lot number 20140103.Injection liquid of gentamicin Kunming Medicine Stock Co., Ltd product, lot number
20140105。
2nd, strain：Staphylococcus aureus, proteus, Pseudomonas aeruginosa, Escherichia coli, by Kunming Medical University's biology
Teaching and research room is learned to provide.
3rd, culture medium：Shanghai medical science assay office provides, lot number 20131205.
Method and result：With cylinder-plate method, 1 as a result see the table below.
The Antimicrobial test table of table 1
Remarks：
(1)1:1、1:5、1:10、1:40 be all weight ratio, i.e. 1g anti-inflammation Chinese medicine suppositories of the present invention respectively with 1g, 1g,
The ratio between 10g, 40g solvent.
(2) in anti-inflammation of the present invention stype liquid preparation：By the preparation of the need testing solution of " alum assay " item
It is prepared by method.
As a result show that anti-inflammation Chinese medicine suppository of the present invention has preferable antibacterial action to above-mentioned common pathogen.
B, the anastalsis of anti-inflammation Chinese medicine suppository
Experiment material
1st, animal：Mouse ICR/JCL strains, provided by natural drug emphasis pharmacological room of Kunming Medical University.
2nd, medicine：Radix Notoginseng powder, commercially available, it is 5% suspension that the used time, which is configured to weight/mass percentage composition,.Evans blue pulvis, English
BDH companies of state produce, and it is 0.5% Evans blue normal saline solution that the used time, which is configured to weight/mass percentage composition,.Antibacterial of the present invention disappears
Scorching Chinese medicine suppository, lot number 20140101.
Method and result：
1st, influence (docking method) of the anti-inflammation Chinese medicine suppository to the mouse bleeding time
From healthy mice 80,18~22g of body weight, male and female dual-purpose, 4 groups are randomly divided into.
Control group：To taking drinking water (0.2ml/20g).
Radix Notoginseng powder group：(1g/kg).
Anti-inflammation Chinese medicine suppository high dose group：(1g/kg).
Anti-inflammation Chinese medicine suppository low dose group：(0.5g/kg).
Daily each group mouse stomach is administered once, continuous three days, after last dose one hour, imitates Ministry of Public Health's medicine management
Office：The method of the drug efficacy study citing 1994.172 of study of tcm new drug guide chapter 4 Chinese medicine, each group mouse is determined respectively and is broken
Tail bleeding time, the data obtained carry out significance test with control group, the results are shown in Table 2.
Influence of the table 2 to mouse bleeding stopping period
As a result show that anti-inflammation Chinese medicine suppository of the present invention can significantly shorten the mouse docking time.
2nd, influence (slide method) of the anti-inflammation Chinese medicine suppository to clotting time of mice
Mouse condition：Packet and administering mode are same as above, and 1 hour after each medicine of last, are imitated《Pharmacological experiment study course is revised
Version》(Guizhou People's Press summer handle nanmu etc. 1986102~104) method, extracing side eyeball with the curved tweezer of ophthalmology makes drop of blood in load
On slide, respectively determine each group clotting time of mice, the data obtained take statistics processing, the results are shown in Table 3.
Influence (slide method) of the table 3 to clotting time of mice
As a result show that anti-inflammation Chinese medicine suppository of the present invention can significantly shorten clotting time of mice
C, influence of the anti-inflammation Chinese medicine suppository to chmice acute experimental inflammatory
1st, the influence of mice auricle swelling caused by paraxylene
Comparative example 1
The difference of comparative example 1 and embodiment 5 is not add borneol, and remaining is all identical.
Comparative example 2
The difference of comparative example 2 and embodiment 5 is not add polyoxyethylene sorbitan monoleate, and remaining is all identical.
Comparative example 3
What the difference of comparative example 3 and embodiment 5 was to prepare is parenteral solution, i.e., raw material is only from alum 50g, fibrauretine
10g and red halloysite 40g, parenteral solution is prepared into according to conventional method in pharmacopeia, and active constituent content is same as Example 5.
This item is tested in addition to positive controls mouse gives aspirin (0.2g/kg), and remaining packet administration is same as above, and is contrasted
Example 1-3 product groups dosage is 1g/kg.Dimethylbenzene 0.05ml causes are respectively applied within 1 hour after this administration on mouse right ear two sides
It is swollen, cervical vertebra is taken off after 15 minutes and puts to death animal, is imitated《The antiinflammatory action of 3-acetylaconitine》Method【Acta Pharmacologica Sinica 1984.5
(2)85-89】With 6mm card punch along left and right auricle same area punch draw materials, weigh respectively, using two auricle method of double differences values as swell
Swollen level index, the difference between more each medicine group and drinking water control group, as a result see the table below 4.
The paraxylene of table 4 causes the influence of mice auricle swelling
2nd, Dichlorodiphenyl Acetate stimulates the influence for causing abdominal cavity capillary permeability
From male mice, packet and administration are same as above method.In last dose 1 hour, each group mouse tail vein injection quality
Percentage composition is 0.5% Evans blue normal saline solution 0.1ml/10g, and after 5 minutes, intraperitoneal injection weight/mass percentage composition is
0.7% acetic acid 0.1ml/10g, after 30 minutes, neck is drawn to put to death mouse.With physiological saline, abdominal cavity is rinsed by several times, merges washing lotion, and
10ml is diluted to, centrifugation 15 minutes (3000 revs/min) takes supernatant, with 721 type spectrophotometers in 690nm wavelength colorimetrics, institute
Obtain OD value and the micrograms of the Evans blue oozed out in every mouse peritoneal are found on standard curve, and at take statistics
Reason, as a result see the table below 5.
The Dichlorodiphenyl Acetate of table 5 stimulates the influence for causing abdominal cavity capillary permeability
Two groups of experimental results of the above show that it is experimental that anti-inflammation Chinese medicine suppository of the present invention can significantly inhibit chmice acute
Inflammatory reaction.
Clinical trial：
(1) 1000 different symptoms oral inflammation patients are selected at random, using product of the present invention, wherein the people of male patient 520,
The people of female patient 480, the oldest patient 65 years old, minimum 16 years old, wherein effective 990 people, obvious effective rate 99%.Using rear effective
Symptom improves after 2-3 days faster, consolidates 1-2 days, and symptom disappears, and does not recur；Effective slower, symptom subtracts after 5 days after use
Gently, consolidate 2-5 days, symptom disappears, and does not occur allergy or obvious gastrointestinal side effect.
(2) it is specific such as table 6 using product of the present invention to the patient with different inflammatory diseases.
Table 6
Claims (4)
1. a kind of anti-inflammation Chinese medicine suppository, it is characterised in that including following component in parts by weight：
Alum 48-52 parts, fibrauretine 8-12 parts, red halloysite 38-42 parts, borneol 8-12 parts, polyoxyethylene sorbitan monoleate 18-22 parts, glycerine
Gelatin is 900-920 parts；
Preparation process is as follows：
Step（1）, alum, red halloysite and borneol are respectively crushed into fine powder；
Step（2）, fibrauretine is crossed 100 mesh sieves；
Step（3）, take red halloysite fine powder to add water for injection 390-410 parts, adjust pH to 3.0 with watery hydrochloric acid, heating is boiled, and is boiled
Boiling 1 hour, then stop heating, after being cooled to room temperature, standing makes insoluble matter fully precipitate, and takes supernatant and filters, obtains clear
Clear filtrate；
Step（4）, step（3）Obtained clear filtrate is heated to boiling, and then adds alum fine powder, and stirring makes to be completely dissolved,
Filter while hot, filtrate is then concentrated into 49-51 parts, be cooled to 50-60 DEG C, and maintain the temperature at 50-60 DEG C；
Step（5）, glycerin gelatine is heated to 50-60 DEG C, is completely melt it, is then slowly added into step while stirring（4）
The solution of gained, fibrauretine, borneol fine powder and the polyoxyethylene sorbitan monoleate for having crossed 100 mesh sieves, stir to well mixed, reverse mould granulation,
Cooling, packaging, that is, obtain anti-inflammation Chinese medicine suppository.
2. anti-inflammation Chinese medicine suppository according to claim 1, it is characterised in that as follows including in parts by weight
Component：
50 parts of alum, 10 parts of fibrauretine, 40 parts of red halloysite, 10 parts of borneol, 20 parts of polyoxyethylene sorbitan monoleate, glycerin gelatine 900-920
Part.
3. anti-inflammation Chinese medicine suppository according to claim 1, it is characterised in that step（3）Described time of repose is
24 hours.
4. according to the detection method of anti-inflammation Chinese medicine suppository made from the preparation method of claim 1, it is characterised in that including
Following steps：
First, character detection：Anti-inflammation Chinese medicine suppository is the bolt of yellow；
Second, differentiate：
The preparation of need testing solution：Anti-inflammation Chinese medicine suppository is taken, is put in evaporating dish, is heated to melting in water-bath, and constantly stir
To mix, make to be well mixed, cool down, precision weighs 10g, put in 100ml measuring bottles, adds methanol 80-85ml, put in 50 DEG C of water-baths and heat,
After constantly shaking makes dissolving, then shake 5 minutes, let cool, with methanol dilution to scale, shake up, filter, discard coarse filtration liquid, it is accurate
Subsequent filtrate 10ml is measured, is put in 100 ml measuring bottles, is 70% methanol dilution to scale with volume fraction, shakes up, filter membrane filtration, i.e.,
Obtain need testing solution；
A. the detection of alum
Need testing solution 2ml is taken, to gelatinous precipitate is generated sodium alizarine sulphonate test solution is added dropwise few drops in ammonification test solution, and it is red to precipitate aobvious cherry
Color；
B. the thin-layer chromatography detection of the palmatin hydrochloride in fibrauretine
Take need testing solution；Palmatin hydrochloride reference substance separately is taken, adds ethanol that solution of every 1ml containing 0.1mg is made, as reference substance
Solution；According to《Chinese Pharmacopoeia》The B thin-layered chromatography of one annex of version in 2010 VI test, draw respectively above-mentioned need testing solution and
Each 5ul of reference substance solution, put respectively on same silica gel g thin-layer plate, using volume ratio as 7:1:2 isoamyl acetate-anhydrous second
The mixed solvent of alcohol-formic acid is solvent, is deployed, and takes out, dries, put under uviol lamp, inspected in 365um, in test sample chromatogram
On position corresponding with reference substance chromatogram, show the fluorescence spot of identical color；
C. the detection of borneol
Take need testing solution 1ml, 1% vanillin-sulfuric acid solution 3-5 drops of dropwise addition, i.e., aobvious purple；
3rd, content detection：
（1）, fibrauretine assay
According to《Chinese Pharmacopoeia》The attached VI D high effective liquid chromatography for measuring of version one in 2010；
Chromatographic condition and system suitability：It is filler with octadecylsilane chemically bonded silica；Using volume ratio as 30:70:0.2
The mixed solvent of acetonitrile-water-phosphoric acid is mobile phase；Flow velocity is 1.0ml/min, and column temperature is that 30 DEG C of Detection wavelengths are 272nm, theoretical
Plate number is calculated by palmatin hydrochloride peak should be not less than 1800；
The preparation of reference substance solution：Palmatin hydrochloride reference substance is taken, adds 70% methanol that solution of every 1ml containing 70ug is made, produces；
The preparation of need testing solution：Anti-inflammation Chinese medicine suppository is taken, is put in evaporating dish, is heated to melting in water-bath, and constantly stir
To mix, make to be well mixed, cool down, precision weighs 10g, put in 100ml measuring bottles, adds methanol 80-85ml, put in 50 DEG C of water-baths and heat,
After constantly shaking makes dissolving, then shake 5 minutes, let cool, with methanol dilution to scale, shake up, filter, discard coarse filtration liquid, it is accurate
Subsequent filtrate 10ml is measured, is put in 100 ml measuring bottles, is 70% methanol dilution to scale with volume fraction, shakes up, filter membrane filtration, i.e.,
Obtain need testing solution；
Determination method：It is accurate respectively to draw reference substance solution and each 10ul of need testing solution, liquid chromatograph is injected separately into, is determined,
Produce；
Anti-inflammation Chinese medicine suppository is containing fibrauretine with palmatin hydrochloride（C21H21NO4·HCl）Calculate, should be the 70- of labelled amount
115%；
（2）Alum assay
The preparation of need testing solution：Anti-inflammation Chinese medicine suppository is taken, is shredded, is mixed, precision weighs 5g, puts in 50ml measuring bottles, add
Water is put in 60-65 DEG C of water-bath, shaking makes dissolving, then takes out and lets cool, be diluted with water to scale, shakes up, and filters, abandons to 40ml
Coarse filtration liquid is gone, subsequent filtrate is put in measuring bottle, is produced；
Precision draws need testing solution 20ml, adds the ml of acetic acid-ammonium acetate buffer 20 that pH is 6.0, then add 0.05mol/L's
The acetic acid disodium titrating solution 25ml of two ammonium of second four, heating are boiled, boil 8-10 minutes, let cool, and add xylenol orange indicator solution 1ml, are used
0.05mol/L zinc titrating solution is titrated to solution and is changed into red from yellow, and the result of titration is corrected with blank test；Often
Aqueous sulfuric acid aluminium potassium [KAl (SO of the 1ml 0.05mol/L acetic acid disodium titrating solution of two ammonium of second four equivalent to 23.72mg4)2·
12H2O]；
Anti-inflammation Chinese medicine suppository is containing alum with aqueous sulfuric acid aluminium potassium [KAl (SO4)2·12H2O] calculate, it should be labelled amount
80%-120%。
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| CN105311568A (en) * | 2015-11-19 | 2016-02-10 | 郝艳 | Traditional Chinese medicinal liquor for relieving swelling |
| CN105311430A (en) * | 2015-11-19 | 2016-02-10 | 郝艳 | Traditional Chinese medicine with inflammation-diminishing effect and antibody |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1279987A (en) * | 2000-06-26 | 2001-01-17 | 凌朝坤 | Medicine for curing piles |
| CN1772239A (en) * | 2005-08-10 | 2006-05-17 | 徐小岗 | Chinese medicine prepn for treating vaginitis and cervicitis |
| CN102727634A (en) * | 2011-04-02 | 2012-10-17 | 于邈 | Traditional Chinese medicine composition for treating gynecological disease |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1062740C (en) * | 1995-10-31 | 2001-03-07 | 赵树生 | Suxiaozhi injection liquid for haemorrhoids and preparation thereof |
| CN1272038C (en) * | 2005-02-02 | 2006-08-30 | 广西康华药业有限责任公司 | Preparation of Chinese medicinal suppository for treating female chronic cervicitis |
| CN1857305A (en) * | 2006-03-10 | 2006-11-08 | 郭凌云 | Pile-treating Fanteng preparation and its preparing process |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1279987A (en) * | 2000-06-26 | 2001-01-17 | 凌朝坤 | Medicine for curing piles |
| CN1772239A (en) * | 2005-08-10 | 2006-05-17 | 徐小岗 | Chinese medicine prepn for treating vaginitis and cervicitis |
| CN102727634A (en) * | 2011-04-02 | 2012-10-17 | 于邈 | Traditional Chinese medicine composition for treating gynecological disease |
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