CN100453114C - Composition of Chinese traditional medicine for treating cold in virulence, and preparation method - Google Patents
Composition of Chinese traditional medicine for treating cold in virulence, and preparation method Download PDFInfo
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Abstract
The present invention discloses a medicine composition for treating viral colds and a preparation method thereof. The medicine composition for treating viral colds is mainly prepared from eleven kinds of medicines, such as isatis roots, gypsum, unprocessed rehmannia roots, cablin patchouli herbs, fructus forsythiae, reed rhizomes, curcuma roots, grassleaved sweetflag rhizomes, anemarrhenae, sucrose, aspartame, citric acid, sodium alginate and potassium sorbate. The present invention is manufactured into clinical acceptable gel preparation by adding pharmaceutical acceptable excipient directly or indirectly by adopting a conventional technique, and the present invention has the functions of clearing heat, expelling damp, removing heat from the blood and detoxicating.
Description
Technical field
The present invention relates to a kind of Chinese medicine composition and preparation method thereof and quality determining method, osteoporotic Chinese medicine composition of particularly a kind of treatment and preparation method thereof and quality determining method.
Background technology
Flu is common exterior syndromes of the four seasons, sees with winter and spring especially more.Many families all have the Chinese patent medicine of treatment flu, eaten many medicines after the somebody catches a cold, but disease do not alleviate.Key is there is not diagnosis and prescription.The traditional Chinese medical science thinks that flu generally can be divided into anemofrigid cold and anemopyretic cold two big classes.These two kinds flu etiology and pathogenesis, symptom, Therapeutic Principle and medication difference are very big.
Anemopyretic cold is due to evil criminal's table, the lung qi of wind heat become estranged.Symptom shows as heating weight, micro evil wind, distending pain in the head, antiperspirant, red swelling and pain of throat, cough, expectorant sticking or yellow, have a stuffy nose yellow thick nasal discharge, thirst and liking drink, red, the little Huang of white and thin fur in the tip of the tongue limit is arranged.Method of treatment should be based on relieving the exterior syndrome with drugs of pungent in flavor and cool in nature.
The medicine that contains aminophenazone, dipyrone, phenacetin etc. in the present coldrex is more, though effective antipyretic analgesic makes the people temporarily feel more comfortable, untoward reaction is arranged.The former two can cause agranulocytosis, immune hemolytic anemia, thrombocytopenic purpura, aplastic anemia etc., and the latter has nephrotoxicity.These survival doses control improperly that thing often has generation, when the patient feels that curative effect is unsatisfied with, can independently increase consumption, and untoward reaction unavoidably can take place.Granulocytopenia means the reduction of body immunity.In addition, it also is unscientific only bringing down a fever, and behind the invasion and attack human body of virus, body temperature suitably raises and helps human body that pathogenic factor is brought into play better immunologic function, drives away exopathogen.This two aspects reason has reduced the resistance against diseases of human body.So relatively poor when body constitution, or can cause the state of an illness to increase the weight of during blindly with antipyretic.It is due to patient's inappropriate medication mostly that the state of an illness increases the weight of.
Many people are arranged, even comprise the medical worker,, or just take antimicrobial drug when just cold symptoms having been arranged when throat pain or not in good time.This is an error of principle in fact.The cause of disease of flu is a viral infection, and it is not only invalid to take antimicrobial drug, can also cause virus variation, bacterial resistance, and produce adverse effect.So taking antimicrobial drug, flu many evils are arranged and none benefit.
When the cough symptom is arranged also is wrong with medicine for the treatment of cough and asthma arbitrarily.Cough is that virus itself reaches due to the insecondary stimulation, at first should be at etiological treatment, and simple cough-relieving may be covered the mistake state of an illness.
Antiviral capsules is reliable to the determined curative effect of anemopyretic cold, is comparatively ideal at present curative drug.No obvious toxic-side effects, long-term or repeat to take and do not produce residual hazard and Drug resistance, therefore, we carry out modified form to it, help meeting the need of market and the clinician uses.Change capsule into gel, make mouthfeel better, bioavailability is higher, takes convenient.
Summary of the invention
The object of the invention is to provide the preparation method of a kind of Chinese medicine composition and preparation thereof, and quality determining method that provides this Chinese medicinal composition preparation and uses thereof is provided another purpose of the present invention.
The present invention seeks to be achieved through the following technical solutions:
The raw material of Chinese medicine composition of the present invention is composed as follows:
Radix Isatidis 50-100 weight portion Gypsum Fibrosum 10-60 weight portion Radix Rehmanniae 5-30 weight portion
Herba Pogostemonis 2-30 weight portion Fructus Forsythiae 10-40 weight portion Rhizoma Phragmitis 20-50 weight portion
Radix Curcumae 2-30 weight portion Rhizoma Acori Graminei 2-30 weight portion Rhizoma Anemarrhenae 2-30 weight portion
Sucrose 50-150 weight portion aspartame 0.12 weight portion citric acid 1-4 weight portion
Sodium alginate 2-20 weight portion potassium sorbate 0.12 weight portion.
The preferred weight proportioning of above-mentioned raw materials is as follows:
Radix Isatidis 72 weight portion Gypsum Fibrosum 32 weight portion Radix Rehmanniae 18 weight portions
Herba Pogostemonis 16 weight portion Fructus Forsythiaes 26 weight portion Rhizoma Phragmitiss 34 weight portions
The Radix Curcumae 14 weight portion Rhizoma Acori Graminei 14 weight portion Rhizoma Anemarrhenaes 14 weight portions
Sucrose 100 weight portion aspartames 1.0 weight portion citric acid 2 weight portions
Sodium alginate 11 weight portion potassium sorbate 1.0 weight portions.
The preferred weight proportioning of above-mentioned raw materials is as follows:
Radix Isatidis 60 weight portion Gypsum Fibrosum 55 weight portion Radix Rehmanniae 7 weight portions
Herba Pogostemonis 28 weight portion Fructus Forsythiaes 12 weight portion Rhizoma Phragmitiss 48 weight portions
The Radix Curcumae 6 weight portion Rhizoma Acori Graminei 27 weight portion Rhizoma Anemarrhenaes 7 weight portions
Sucrose 130 weight portion aspartames 0.3 weight portion citric acid 3 weight portions
Sodium alginate 5 weight portion potassium sorbate 1.8 weight portions.
The preferred weight proportioning of above-mentioned raw materials is as follows:
Radix Isatidis 90 weight portion Gypsum Fibrosum 15 weight portion Radix Rehmanniae 25 weight portions
Herba Pogostemonis 7 weight portion Fructus Forsythiaes 35 weight portion Rhizoma Phragmitiss 25 weight portions
The Radix Curcumae 28 weight portion Rhizoma Acori Graminei 5 weight portion Rhizoma Anemarrhenaes 23 weight portions
Sucrose 60 weight portion aspartames 1.7 weight portion citric acid 2 weight portions
Sodium alginate 18 weight portion potassium sorbate 0.3 weight portion.
Chinese medicine composition raw material of the present invention adds according to common process, makes clinical acceptable gel preparation.
The concrete preparation technology of the present composition is as follows:
Get drug regimen raw material of the present invention, the Fructus Forsythiae of Radix Curcumae, Rhizoma Acori Graminei and 50% is placed in the extractor, carry most volatile oil, medicinal liquid filters, and filtrate and volatile oil are standby; The decocting that above residue and Radix Isatidis, Gypsum Fibrosum, Radix Rehmanniae, Rhizoma Phragmitis, the Rhizoma Anemarrhenae five tastes is added 6-10 times of weight portion boils 2-4 time, each 1-2 hour, collecting decoction, filter, filtrate and above-mentioned standby medicinal liquid merge, being condensed into 40 ℃ of-60 ℃ of relative densities is the clear paste of 1.20-1.25, adds the dilution of 400-900 weight parts water, filters; The Fructus Forsythiae powder of Herba Pogostemonis and 50% is broken into fine powder, join in the above-mentioned medicinal liquid, stir evenly, other gets sucrose, aspartame, citric acid and potassium sorbate, add water to dissolving, filter, join in the above-mentioned medicinal liquid, add sodium alginate, add the water stirring and boil the gel that is 1.05-1.25 to 75-95 ℃ of following relative density.
The preferred for preparation technology of the present composition is as follows:
Get drug regimen raw material of the present invention, the Fructus Forsythiae of Radix Curcumae, Rhizoma Acori Graminei and 50% is placed in the extractor, carry most volatile oil, medicinal liquid filters, and filtrate and volatile oil are standby; The decocting that above residue and Radix Isatidis, Gypsum Fibrosum, Radix Rehmanniae, Rhizoma Phragmitis, the Rhizoma Anemarrhenae five tastes is added 9 times of weight portions boils 3 times, each 1.5 hours, collecting decoction, filter, filtrate and above-mentioned standby medicinal liquid merge, does the clear paste that to be condensed into 50 ℃ of relative densities be 1.20-1.25 add 800 weight portions? the water dilution filters; The Fructus Forsythiae powder of Herba Pogostemonis and 50% is broken into fine powder, join in the above-mentioned medicinal liquid, stir evenly, other gets sucrose, aspartame, citric acid and potassium sorbate, add water to dissolving, filter, join in the above-mentioned medicinal liquid, add sodium alginate, adding that water stirs and boil to 80 ℃ of following relative densities is 1.10 gel.
Quality determining method of the present invention comprises following discrimination method and/or content assaying method
Discrimination method comprises a kind of and/or several in the following discriminating:
A. get this pharmaceutical composition, be ground into pulpous state, get 20g, add water 100ml, reflux 30 minutes filters, and filtrate is transferred pH to 2 with 6mol/L hydrochloric acid, extracts with ether 20ml, reclaims ether, and residue adds dehydrated alcohol 0.5ml makes dissolving, as test sample; Other evens up pier fruit acid reference substance, adds dehydrated alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to the test of thin chromatography, draw each 5 μ l of above-mentioned solution, put respectively in same be the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with 10: 1 chloroform-methanols, launch, take out, dry; Spray is with 10% sulfuric acid solution, and it is clear to dry by the fire to the speckle colour developing at 105 ℃; In the test sample chromatograph, with reference substance chromatograph relevant position on, should show the speckle of same color;
B. get this pharmaceutical composition, be ground into pulpous state, get 30g, add 60-90 ℃ of petroleum ether 300ml, reflux 30 minutes filters, and reclaims solvent, and residue adds cyclohexane extraction 1ml makes dissolving, as need testing solution; Other gets Herba Pogostemonis control medicinal material 0.5g, gets control medicinal material solution with legal system; According to the test of thin chromatography, draw each 10 μ l of above-mentioned solution, put respectively in same be the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with 10: 1 60-90 ℃ petroleum ether-ethyl acetate, launch, take out, dry; Spray is with 5% anisaldehyde sulfuric acid solution, and it is clear to dry by the fire to the speckle colour developing in 110 ℃; In the test sample chromatograph, with reference substance chromatograph relevant position on, should show the speckle of same color;
C. get this pharmaceutical composition, be ground into pulpous state, get 10g, add Diluted Alcohol 100ml, 350W, 50KHz supersound process 30min takes out, and puts coldly, filters, and evaporate to dryness, residue add Diluted Alcohol 5ml dissolving, as need testing solution; It is an amount of that other gets the arginine reference substance, adds Diluted Alcohol and make the solution that every 1ml contains 0.2mg, in contrast product solution; According to the test of thin chromatography, draw each 5 μ l of above-mentioned solution, put respectively in same be the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with 19: 5: 5 n-butyl alcohol-glacial acetic acid-water, launch, take out, dry; Spray is with ninhydrin solution, and it is clear to dry by the fire to the speckle colour developing in 105 ℃; In the test sample chromatograph, with reference substance chromatograph relevant position on, should show the speckle of same color.
Content assaying method in the quality determining method is as follows:
According to high effective liquid chromatography for measuring; Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; 87: 13: 0.1 methanol-water-phosphoric acid are mobile phase; The detection wavelength is 208nm; Number of theoretical plate calculates by the oleanolic acid peak should be not less than 3000; The preparation of reference substance solution: it is an amount of that precision takes by weighing the oleanolic acid reference substance, adds methanol and make the solution that every 1ml contains 0.1mg, promptly; The preparation of need testing solution: sample thief is an amount of, is ground into pulpous state, gets about 10g, the accurate title, decide, and adds methanol 200ml, reflux 2 hours, filter, the medicinal residues methanol wash, washing liquid is incorporated filtrate into, reclaim methanol, the residue dissolve with methanol, transfer and standardize solution are to the 10ml measuring bottle, shake up, cross 0.45 μ m microporous filter membrane, get subsequent filtrate, promptly; Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
Gel of the present invention not only contains the active component of dose therapeutically effective, simultaneously because the improvement of mouthfeel has strengthened the compliance of drug administration.Anti-virus formulation is mainly used in the treatment anemopyretic cold, diseases such as pestilence heating and upper respiratory tract infection, influenza, parotitis.Upper respiratory tract infection, influenza, parotitis are modal diseases in children's's period.At present, existing anti-virus formulation has capsule, tablet, granule, oral liquid, and children's swallows and can have any problem when taking above-mentioned tablet, capsule, and capsule broken into two with one's hands or slice, thin piece pulverized after take, the poor taste of medicated powder can make children's be difficult to swallow again.Because main component all is dissolved in the solution, the taste of some composition was difficult to cover, and makes the child be unwilling to take when granule and oral liquid were taken.We have made the fruit jelly gel that liked by the child on the basis of original prescription, because active component in gel-type vehicle, has been covered disagreeable taste, it is good in mouthfeel when the patient takes, taste is suitable, and children's extremely is ready to take, and has improved the compliance of medication in children.
Following experiment and embodiment are used to further specify but are not limited to the present invention.
The experiment of experimental example 1 Study on extraction process
1, three flavor volatile oil such as Radix Curcumae extract trial tests
Take by weighing Radix Curcumae 70g, Rhizoma Acori Graminei 70g, Fructus Forsythiae 65g, add 10 times of water gagings and soaked 3 hours, continuous backflow was extracted 6 hours, collected volatile oil, saltout volatile oil 2.09g.
Find in the process of the test that the amount of extracting volatile oil after 6 hours does not almost change, and can think and extract after 6 hours that volatile oil has extracted and finished.
By trial test as can be known, influencing factor that volatile oil extracts has the water of adding doubly amount, soak time, extraction time etc., and these factors will be discussed in orthogonal test.
2, volatile oil extracts orthogonal test
Take by weighing Radix Curcumae 70g, Rhizoma Acori Graminei 70g, Fructus Forsythiae 65g, be total to 205g, nominal is got nine parts, presses L9 (3
4) orthogonal table, add the water reflux, extract, respectively, collect volatile oil, saltout, claim the volatilization oil mass, investigate for the ease of the data on the statistics, the index amount is enlarged 20 times, result of the test is as follows:
Table 1 volatile oil extracts orthogonal test factor level table
Table 2 orthogonal array and index determining be table as a result
Table 3 variance of totals analytical table
F
1-0.01(2，2)＝99；F
1-0.05(2，2)＝19；F
1-0.10(2，2)＝9
Above-mentioned orthogonal experiments shows that the factor primary and secondary that the volatilization oil mass is influenced is C＞A＞B in proper order; A factor (adding water doubly measures) and B factor (soak time), variant F
1-0.10(2,2)＜F＜F
1-0.05(2,2), on average, 2 levels of A factor and B factor and 3 levels respectively near and all greater than 1 level, consider to conserve water and economize factor such as energy when saving, select A respectively
2And B
2, promptly add 10 times of water gagings and immersion 2 hours; C factor (extraction time) has significant difference F＞F
1-0.01(2,2), on average, C
2And C
3Near and all greater than C
1, economize factors such as energy when considering joint, so select C
2, promptly extracted 6 hours.Therefore, comprehensive above various factors considers that the preferable extraction process of determining is A
2B
2C
2, promptly Radix Curcumae, Rhizoma Acori Graminei, Fructus Forsythiae add 10 times of water gagings immersions 2 hours, and continuous backflow was extracted 6 hours, collected volatile oil.
3, volatile oil extracts demonstration test: take by weighing Radix Curcumae 70g, Rhizoma Acori Graminei 70g, Fructus Forsythiae 65g, add 10 times of water gagings and soaked 2 hours, continuous backflow was extracted 6 hours, collected volatile oil, saltout volatile oil, result of the test is as follows:
Table 4 volatile oil is carried demonstration test table as a result
Brief summary: can find out by the demonstration test result, three result of the test opposing parallel, technology has repeatability preferably; Therefore determine that the volatile oil extraction process is: Radix Curcumae, Rhizoma Acori Graminei, Fructus Forsythiae add 10 times of water gagings and soaked 2 hours, and continuous backflow was extracted 6 hours, collect volatile oil.
4, water extraction is to demonstration test when
Take by weighing the medical material of antiviral capsules 1/4 recipe quantity, totally nine parts, Radix Curcumae 17.5g, Rhizoma Acori Graminei 17.5g, Fructus Forsythiae 16.25g add 10 times of water gagings and soaked 2 hours, and continuous backflow was extracted 6 hours, and medicinal liquid filters, filtrate for later use; The five tastes such as medicinal residues and Radix Isatidis 90g, Gypsum Fibrosum 40g, Radix Rehmanniae 22.5g, Rhizoma Phragmitis 42.5g, Rhizoma Anemarrhenae 17.5g decoct with water three times, for the first time, each 2 hours for the second time, 1 hour for the third time, collecting decoction, filter, filtrate and above-mentioned standby medicinal liquid merge, and being condensed into relative density is the clear paste of 1.20-1.25 (50 ℃ of surveys), claim the clear paste amount, vacuum drying then, and with dried cream amount as controlling index, doubly measure and carry out preferably adding water, result of the test is as follows:
Table 5 water extraction is to demonstration test result when
By water extraction to demonstration test result when as can be known, adding the result that 6,8,10 times of water gagings extract does not have significant difference, economizes factors such as energy when considering in the actual production joint, chooses to add 6 times of water gagings and extract; 1,2, No. 3 result of the tests show, three result of the tests that add 6 times of water gagings extractions do not have significant difference yet, have repeatability preferably; Therefore determine that water extraction process for the Fructus Forsythiae with Radix Curcumae, Rhizoma Acori Graminei and 50% places in the extractor, adds 10 times of water gagings and soaked 2 hours, continuous backflow was extracted volatile oil 6 hours, and medicinal liquid filters, and filtrate and volatile oil are standby; The five tastes such as above residue and Radix Isatidis, Gypsum Fibrosum, Radix Rehmanniae, Rhizoma Phragmitis, the Rhizoma Anemarrhenae are added 6 times of water gagings decoct three times, for the first time, each 2 hours for the second time, 1 hour for the third time, collecting decoction filtered, and filtrate merges concentrated with above-mentioned standby medicinal liquid.
Experimental example 2 prescription screening research experiments
1, the test of the addition of citric acid and sodium alginate
For determining the amount of sodium alginate, do the preliminary preparation of gel, get the 18g clear paste for every part, 2.72g medical material fine powder, clear paste add suitable quantity of water and stir, and filter, and add the medical material fine powder again, stir.Add citric acid, mouth is tasted its flavor, adds Icing Sugar, sodium alginate and potassium sorbate again, adds water to 100g (every bag is equivalent to the 10g gel), and 40-60min is also stirred in 80-90 ℃ of insulation, takes out, and cools off under the room temperature, observes gel forming situation and trial test taste.The results are shown in following table:
The result of the test of the addition of table 6 citric acid and sodium alginate
Conclusion: when medicinal liquid added 0.2% citric acid, mouth was tasted medicinal liquid, and little acid of distinguishing the flavor of continues to add citric acid again and is unfavorable for that the molding of gel and part crowd are difficult for accepting; When medicinal liquid added 1.1% sodium alginate, therefore the gel that makes neither too hard, nor too soft determined that the addition of citric acid is 0.2%, and the addition of sodium alginate is 1.1%, and every bag is equivalent to the 10g gel.
2, the screening of sweeting agent
All get the 18g clear paste for every part, add suitable quantity of water and stir, filter, add 2.72g medical material fine powder again, stir, add Icing Sugar, aspartame, citric acid successively, mouthful gustation road according to following table, the good person of selected part taste adds sodium alginate and potassium sorbate, add water to 100g, 80-90 ℃ of insulation also stirred 40-60min, takes out, cool off under the room temperature, observe the character of gel and taste taste.
Table 7 prescription screening table (10 bags every part, 100g)
Conclusion: 1, do not add sodium alginate and potassium sorbate No. 2, tentatively investigate mouthfeel, 3,4, No. 5 test specimens all add sodium alginate and potassium sorbate is made gel, No. 5 mouthfeel is better, and mildly bitter flavor, sweet is little puckery, take all factors into consideration, finally select No. 5 prescriptions to be this product preparation prescription.
The experiment of experimental example 3 technology repeatability
Recipe quantity by 1000g feeds intake three batches, carries out the test of technology repeatability.
Prescription:
Radix Isatidis 72g Gypsum Fibrosum 32g Radix Rehmanniae 18g
Herba Pogostemonis 16g Fructus Forsythiae 26g Rhizoma Phragmitis 34g
Radix Curcumae 14g Rhizoma Acori Graminei 14g Rhizoma Anemarrhenae 14g
Method for making: above nine flavors, the Fructus Forsythiae of Radix Curcumae, Rhizoma Acori Graminei and 1/2nd recipe quantities is placed in the extractor, add 10 times of water gagings and soaked 2 hours, continuous backflow was extracted volatile oil 6 hours, and medicinal liquid filters, and filtrate and volatile oil are standby; The five tastes such as above residue and Radix Isatidis, Gypsum Fibrosum, Radix Rehmanniae, Rhizoma Phragmitis, the Rhizoma Anemarrhenae are added 6 times of water gagings to be decocted three times, each 2 hours for the second time for the first time,, 1 hour for the third time, collecting decoction, filter, filtrate and above-mentioned standby medicinal liquid merge, and being condensed into relative density is the clear paste of 1.20-1.25 (50 ℃ of surveys), add the suitable quantity of water dilution, filter; The Fructus Forsythiae powder of Herba Pogostemonis and 1/2nd recipe quantities is broken into fine powder, joins in the above-mentioned medicinal liquid, stir evenly, other gets sucrose, aspartame, citric acid and potassium sorbate, adds the suitable quantity of water heating for dissolving, filters, join in the above-mentioned medicinal liquid, add sodium alginate, fully stir, supply water to ormal weight, stirring is also boiled, and 80-90 ℃ of insulation adds volatile oil and fill in good time, every packed 10g, promptly.
Table 8 technology repeatability experimental result table (1000g, 100 bags)
By table 8 experimental result as can be known, the preparation technology by fixed gel of the present invention has carried out the preparation of three batches of gel samples of the present invention, and every index basically identical of sample shows that this prescription and technology have repeatability preferably.
The assay experimentation of experimental example 4 oleanolic acid
1, chromatographic condition determines
(1), the selection of wavelength
It is an amount of to take by weighing the oleanolic acid reference substance, adds methanol and makes the solution that every 1ml contains 0.2mg, in the wave-length coverage interscan of 200nm-400nm.The result shows that this product has maximum absorption wavelength at the 208nm place.Select the detection wavelength of 208nm as this product.
(2), the selection of mobile phase
Through consulting documents and materials, in conjunction with the characteristics of this product, through groping in many ways, selecting methanol-water-phosphoric acid (87: 13: 0.1) is mobile phase in the test.
The result shows that main peak and other peak energy reach baseline separation, and appearance time is suitable.Methanol-water-phosphoric acid (87: 13: 0.1) is suitable as the assay method of this product.
(3), chromatographic condition
Chromatographic column: octadecylsilane chemically bonded silica post (5 μ m, 4.6 * 250mm)
Detect wavelength: 208nm
Mobile phase: methanol-water-phosphoric acid (87: 13: 0.1)
Column temperature: room temperature
Flow velocity: 1.0ml/min
2, extracting method determines
(1), extracts choice of Solvent
It is an amount of to get this product, is ground into pulpous state, and precision takes by weighing 6 parts, every part of about 10g, the accurate methanol 200ml that adds of first and second part, the accurate ether 200ml that adds of third and fourth part, five, six parts of accurate chloroform 200ml that add, reflux is 3 hours respectively, puts cold, filter, residue with separately solvent wash 3 times, is reclaimed solvent, residue adds an amount of dissolve with methanol, transfers in the 10ml measuring bottle and is diluted to scale, shakes up, cross 0.45 μ m filter membrane, get subsequent filtrate, promptly.It is an amount of that other evens up pier fruit acid reference substance, adds methanol and make the solution that every 1ml contains 0.1mg, in contrast product solution.
Accurate each the 10 μ l of above-mentioned solution that draw inject chromatograph of liquid, measure by the chromatographic condition of drafting, and the results are shown in Table 9.
The result that table 9 different solvents extracts
According to the result, selecting methanol is the extraction solvent of this experiment.
(2), the selection of extracting method
It is an amount of to get this product, is ground into pulpous state, and precision takes by weighing 4 parts, every part of about 10g, accurate methanol 200ml, first and second part reflux 3 hours of adding, third and fourth part supersound process (power 350W, frequency 50kHz) 2 hours filters, with residue methanol wash 3 times, reclaim methanol, residue adds an amount of dissolve with methanol, transfer in the 10ml measuring bottle and be diluted to scale, shake up, cross 0.45 μ m filter membrane, get subsequent filtrate, promptly.It is an amount of that other evens up pier fruit acid reference substance, adds methanol and make the solution that every 1ml contains 0.1mg, in contrast product solution.
Accurate each the 10 μ l of above-mentioned solution that draw inject chromatograph of liquid, measure by the chromatographic condition of drafting, and the results are shown in Table 10.
The selection of table 10 extracting method
According to result of the test, select reflux as extracting method.
(3), the investigation of extraction time
It is an amount of to get this product, is ground into pulpous state, and precision takes by weighing 6 parts of this product, every part of about 10g, accurate respectively methanol 200ml, reflux, first and second part 1 hour of adding, third and fourth parts 2 hours, the 5th, six part 3 hours, put cold, filter,, reclaim methanol residue methanol wash 3 times, residue adds an amount of dissolve with methanol, transfers in the 10ml measuring bottle and is settled to scale, shakes up, cross 0.45 μ m filter membrane, get subsequent filtrate, promptly.It is an amount of that other evens up pier fruit acid reference substance, adds methanol and make the solution that every 1ml contains 0.1mg, in contrast product solution.
Accurate each the 10 μ l of above-mentioned solution that draw inject chromatograph of liquid, measure by the chromatographic condition of drafting, and the results are shown in Table 11.
The result of the different extraction times extractions of table 11
According to result of the test, take all factors into consideration test period and experimentation cost, select to be in 2 hours the extraction time of this experiment at last.
(4), negative interference experiment
Take by weighing all the other flavour of a drug except that Fructus Forsythiae in the prescription ratio, make negative sample by preparation technology.Make the negative solution that lacks Fructus Forsythiae by the preparation method of test sample.
Draw negative solution 10 μ l sample introductions, observe whether impurity peaks is arranged at the retention time place at sample peak.
Record the result and show, do not have obvious impurity peaks at sample retention time place and disturb.
(5), need testing solution preparation
It is an amount of to get this product, is ground into pulpous state, and precision takes by weighing about 10g, the accurate methanol 200ml that adds, reflux 2 hours is put cold, filter, methanol is reclaimed in medicinal residues methanol wash 3 times, residue adds an amount of dissolve with methanol, transfer in the 10ml measuring bottle and be diluted to scale, shake up, cross 0.45 μ m filter membrane, get subsequent filtrate, promptly.
3, methodological study
(1), linear relationship investigates accurate reference substance solution (0.02412mg/ml) 1,2,4,6, the 8 μ l that draw, and puts in the 10ml measuring bottle, adds methanol and is diluted to scale, shake up, promptly.Measuring peak area by the chromatographic condition of drafting, is vertical coordinate with the peak area integrated value, and the amount of oleanolic acid is an abscissa drawing standard curve, calculates regression equation: Y=3168723.7329X-2129.6849r=0.9999.The results are shown in Table 12.
Table 12 linear relationship is investigated
The result shows that oleanolic acid is good linear relationship in the 0.02412-0.2414mg/ml scope.
(2), the precision test is got need testing solution, continuous sample introduction 5 times, each 10 μ l, record chromatogram.Investigate the precision of instrument.The results are shown in Table 13.
Table 13 sample precision experimental result
Above experimental result shows that instrument precision is good.
(3), stability experiment
Get respectively with a need testing solution 10 μ l, measure its peak area at regular intervals, investigate the stability of sample solution, calculate relative standard deviation, the results are shown in Table 14 by above-mentioned chromatographic condition.
Table 14 stability test result
Above experimental result shows that sample is stable in 8 hours.
(4), replica test
Precision takes by weighing (050219) five part in sample, makes need testing solution by the method for working out, and measures peak area by the chromatographic condition of drafting, and calculates content, calculates relative standard deviation＜5%, the results are shown in Table 15.
Table 15 reproducible test results
Conclusion: the repeatability of experiment is good.
(5), average recovery gets five of conical flasks, adds oleanolic acid reference substance solution (0.4524mg/ml) 1ml respectively, evaporate to dryness.Get five parts in the sample of known content, every part of about 5g puts in above-mentioned five conical flasks, makes need testing solution by the need testing solution preparation method, measures by the chromatographic condition of drafting, as follows calculate recovery rate.The results are shown in table 16.
The response rate (%)=(oleanolic acid amount in actual measurement oleanolic acid amount-sample)/interpolation oleanolic acid amount * 100%
Table 16 determination of recovery rates result
The result shows that the response rate of this experiment is good.
4, sample determination
Prepare need testing solution and reference substance solution by the method for drafting, accurate respectively reference substance solution and the need testing solution 10 μ l of drawing inject chromatograph of liquid, measure according to above-mentioned chromatographic condition, calculate content.Sample determination the results are shown in Table 17.
Table 17 sample determination result (n=10)
Tentative this product contains Fructus Forsythiae with oleanolic acid (C for every bag
30H
48O
3) meter, must not be less than 0.60mg.
Description of drawings:
Fig. 1 oleanolic acid is good linear relationship in the 0.02412-0.2414mg/ml scope.
Following embodiment all can realize the effect of above-mentioned experimental example.
The specific embodiment:
Embodiment 1: the preparation of gel
Radix Isatidis 72kg Gypsum Fibrosum 32kg Radix Rehmanniae 18kg
Herba Pogostemonis 16kg Fructus Forsythiae 26kg Rhizoma Phragmitis 34kg
Radix Curcumae 14kg Rhizoma Acori Graminei 14kg Rhizoma Anemarrhenae 14kg
Sucrose 100kg aspartame 1.0kg citric acid 2kg
Sodium alginate 11kg potassium sorbate 1.0kg
Get drug regimen raw material of the present invention, the Fructus Forsythiae of Radix Curcumae, Rhizoma Acori Graminei and 50% is placed in the extractor, carry most volatile oil, medicinal liquid filters, and filtrate and volatile oil are standby; The decocting that above residue and Radix Isatidis, Gypsum Fibrosum, Radix Rehmanniae, Rhizoma Phragmitis, the Rhizoma Anemarrhenae five tastes is added 8-10 times of weight portion boils 2-4 time, each 1-2 hour, collecting decoction, filter, filtrate and above-mentioned standby medicinal liquid merge, being condensed into 40 ℃ of-60 ℃ of relative densities is the clear paste of 1.20-1.25, adds the dilution of 400-900 weight parts water, filters; The Fructus Forsythiae powder of Herba Pogostemonis and 50% is broken into fine powder, join in the above-mentioned medicinal liquid, stir evenly, other gets sucrose, aspartame, citric acid and potassium sorbate, add water to dissolving, filter, join in the above-mentioned medicinal liquid, add sodium alginate, adding that water stirs and boil to 80 ℃ of following relative densities is 1.10 gel.
Embodiment 2: the preparation of gel
Radix Isatidis 60kg Gypsum Fibrosum 55kg Radix Rehmanniae 7kg
Herba Pogostemonis 28kg Fructus Forsythiae 12kg Rhizoma Phragmitis 48kg
Radix Curcumae 6kg Rhizoma Acori Graminei 27kg Rhizoma Anemarrhenae 7kg
Sucrose 130kg aspartame 0.3kg citric acid 3kg
Sodium alginate 5kg potassium sorbate 1.8kg
Get drug regimen raw material of the present invention, the Fructus Forsythiae of Radix Curcumae, Rhizoma Acori Graminei and 50% is placed in the extractor, carry most volatile oil, medicinal liquid filters, and filtrate and volatile oil are standby; The decocting that above residue and Radix Isatidis, Gypsum Fibrosum, Radix Rehmanniae, Rhizoma Phragmitis, the Rhizoma Anemarrhenae five tastes is added 8-10 times of weight portion boils 2-4 time, each 1-2 hour, collecting decoction, filter, filtrate and above-mentioned standby medicinal liquid merge, being condensed into 40 ℃ of-60 ℃ of relative densities is the clear paste of 1.20-1.25, adds the dilution of 400-900 weight parts water, filters; The Fructus Forsythiae powder of Herba Pogostemonis and 50% is broken into fine powder, join in the above-mentioned medicinal liquid, stir evenly, other gets sucrose, aspartame, citric acid and potassium sorbate, add water to dissolving, filter, join in the above-mentioned medicinal liquid, add sodium alginate, adding that water stirs and boil to 85 ℃ of following relative densities is 1.05 gel.
Embodiment 3: the preparation of gel
Radix Isatidis 90kg Gypsum Fibrosum 15kg Radix Rehmanniae 25kg
Herba Pogostemonis 7kg Fructus Forsythiae 35kg Rhizoma Phragmitis 25kg
Radix Curcumae 28kg Rhizoma Acori Graminei 5kg Rhizoma Anemarrhenae 23kg
Sucrose 60kg aspartame 1.7kg citric acid 2kg
Sodium alginate 18kg potassium sorbate 0.3kg
Get drug regimen raw material of the present invention, the Fructus Forsythiae of Radix Curcumae, Rhizoma Acori Graminei and 50% is placed in the extractor, carry most volatile oil, medicinal liquid filters, and filtrate and volatile oil are standby; The decocting that above residue and Radix Isatidis, Gypsum Fibrosum, Radix Rehmanniae, Rhizoma Phragmitis, the Rhizoma Anemarrhenae five tastes is added 8-10 times of weight portion boils 2-4 time, each 1-2 hour, collecting decoction, filter, filtrate and above-mentioned standby medicinal liquid merge, being condensed into 40 ℃ of-60 ℃ of relative densities is the clear paste of 1.20-1.25, adds the dilution of 400-900 weight parts water, filters; The Fructus Forsythiae powder of Herba Pogostemonis and 50% is broken into fine powder, join in the above-mentioned medicinal liquid, stir evenly, other gets sucrose, aspartame, citric acid and potassium sorbate, add water to dissolving, filter, join in the above-mentioned medicinal liquid, add sodium alginate, adding that water stirs and boil to 75 ℃ of following relative densities is 1.08 gel.
Embodiment 4: the preparation of gel
Radix Isatidis 70kg Gypsum Fibrosum 20kg Radix Rehmanniae 25kg
Herba Pogostemonis 4kg Fructus Forsythiae 35kg Rhizoma Phragmitis 30kg
Radix Curcumae 20kg Rhizoma Acori Graminei 10kg Rhizoma Anemarrhenae 18kg
Sucrose 75kg aspartame 1.5kg citric acid 2kg
Sodium alginate 15kg potassium sorbate 0.5kg
Get drug regimen raw material of the present invention, the Fructus Forsythiae of Radix Curcumae, Rhizoma Acori Graminei and 50% is placed in the extractor, carry most volatile oil, medicinal liquid filters, and filtrate and volatile oil are standby; The decocting that above residue and Radix Isatidis, Gypsum Fibrosum, Radix Rehmanniae, Rhizoma Phragmitis, the Rhizoma Anemarrhenae five tastes is added 8-10 times of weight portion boils 2-4 time, each 1-2 hour, collecting decoction, filter, filtrate and above-mentioned standby medicinal liquid merge, being condensed into 40 ℃ of-60 ℃ of relative densities is the clear paste of 1.20-1.25, adds the dilution of 400-900 weight parts water, filters; The Fructus Forsythiae powder of Herba Pogostemonis and 50% is broken into fine powder, join in the above-mentioned medicinal liquid, stir evenly, other gets sucrose, aspartame, citric acid and potassium sorbate, add water to dissolving, filter, join in the above-mentioned medicinal liquid, add sodium alginate, adding that water stirs and boil to 85 ℃ of following relative densities is 1.15 gel.
Embodiment 5: the preparation of gel
Radix Isatidis 80kg Gypsum Fibrosum 20kg Radix Rehmanniae 25kg
Herba Pogostemonis 4kg Fructus Forsythiae 35kg Rhizoma Phragmitis 28kg
Radix Curcumae 25kg Rhizoma Acori Graminei 5kg Rhizoma Anemarrhenae 20kg
Sucrose 60kg aspartame 2kg citric acid 3kg
Sodium alginate 12kg potassium sorbate 2kg
Get drug regimen raw material of the present invention, the Fructus Forsythiae of Radix Curcumae, Rhizoma Acori Graminei and 50% is placed in the extractor, carry most volatile oil, medicinal liquid filters, and filtrate and volatile oil are standby; The decocting that above residue and Radix Isatidis, Gypsum Fibrosum, Radix Rehmanniae, Rhizoma Phragmitis, the Rhizoma Anemarrhenae five tastes is added 8-10 times of weight portion boils 2-4 time, each 1-2 hour, collecting decoction, filter, filtrate and above-mentioned standby medicinal liquid merge, being condensed into 40 ℃ of-60 ℃ of relative densities is the clear paste of 1.20-1.25, adds the dilution of 400-900 weight parts water, filters; The Fructus Forsythiae powder of Herba Pogostemonis and 50% is broken into fine powder, join in the above-mentioned medicinal liquid, stir evenly, other gets sucrose, aspartame, citric acid and potassium sorbate, add water to dissolving, filter, join in the above-mentioned medicinal liquid, add sodium alginate, adding that water stirs and boil to 90 ℃ of following relative densities is 1.05 gel.
Embodiment 6: the discrimination method in the quality testing
A. get the pharmaceutical composition of embodiment 1, be ground into pulpous state, get 20g, add water 100ml, reflux 30 minutes filters, and filtrate is transferred pH to 2 with 6mol/L hydrochloric acid, extracts with ether 20ml, reclaims ether, and residue adds dehydrated alcohol 0.5ml makes dissolving, as test sample; Other evens up pier fruit acid reference substance, adds dehydrated alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to the test of thin chromatography, draw each 5 μ l of above-mentioned solution, put respectively in same be the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with 10: 1 chloroform-methanols, launch, take out, dry; Spray is with 10% sulfuric acid solution, and it is clear to dry by the fire to the speckle colour developing at 105 ℃; In the test sample chromatograph, with reference substance chromatograph relevant position on, should show the speckle of same color;
B. get the pharmaceutical composition of embodiment 1, be ground into pulpous state, get 30g, add 60-90 ℃ of petroleum ether 300ml, reflux 30 minutes filters, and reclaims solvent, and residue adds cyclohexane extraction 1ml makes dissolving, as need testing solution; Other gets Herba Pogostemonis control medicinal material 0.5g, gets control medicinal material solution with legal system; According to the test of thin chromatography, draw each 10 μ l of above-mentioned solution, put respectively in same be the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with 10: 1 60-90 ℃ petroleum ether-ethyl acetate, launch, take out, dry; Spray is with 5% anisaldehyde sulfuric acid solution, and it is clear to dry by the fire to the speckle colour developing in 110 ℃; In the test sample chromatograph, with reference substance chromatograph relevant position on, should show the speckle of same color;
C. get embodiment 1 pharmaceutical composition, be ground into pulpous state, get 10g, add Diluted Alcohol 100ml, 350W, 50KHz supersound process 30min takes out, and puts coldly, filters, and evaporate to dryness, residue add Diluted Alcohol 5ml dissolving, as need testing solution; It is an amount of that other gets the arginine reference substance, adds Diluted Alcohol and make the solution that every 1ml contains 0.2mg, in contrast product solution; According to the test of thin chromatography, draw each 5 μ l of above-mentioned solution, put respectively in same be the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with 19: 5: 5 n-butyl alcohol-glacial acetic acid-water, launch, take out, dry; Spray is with ninhydrin solution, and it is clear to dry by the fire to the speckle colour developing in 105 ℃; In the test sample chromatograph, with reference substance chromatograph relevant position on, should show the speckle of same color.
Embodiment 7: the content assaying method in the quality testing
According to high effective liquid chromatography for measuring; Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; 87: 13: 0.1 methanol-water-phosphoric acid are mobile phase; The detection wavelength is 208nm; Number of theoretical plate calculates by the oleanolic acid peak should be not less than 3000; The preparation of reference substance solution: it is an amount of that precision takes by weighing the oleanolic acid reference substance, adds methanol and make the solution that every 1ml contains 0.1mg, promptly; The preparation of need testing solution: it is an amount of to get embodiment 3 samples, is ground into pulpous state, gets about 10g, the accurate title, decide, and adds methanol 200ml, reflux 2 hours, filter, the medicinal residues methanol wash, washing liquid is incorporated filtrate into, reclaim methanol, the residue dissolve with methanol, transfer and standardize solution are to the 10ml measuring bottle, shake up, cross 0.45 μ m microporous filter membrane, get subsequent filtrate, promptly; Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
Embodiment 8: quality monitoring method
A. get embodiment 2 pharmaceutical compositions, be ground into pulpous state, get 20g, add water 100ml, reflux 30 minutes filters, and filtrate is transferred pH to 2 with 6mol/L hydrochloric acid, extracts with ether 20ml, reclaims ether, and residue adds dehydrated alcohol 0.5ml makes dissolving, as test sample; Other evens up pier fruit acid reference substance, adds dehydrated alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to the test of thin chromatography, draw each 5 μ l of above-mentioned solution, put respectively in same be the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with 10: 1 chloroform-methanols, launch, take out, dry; Spray is with 10% sulfuric acid solution, and it is clear to dry by the fire to the speckle colour developing at 105 ℃; In the test sample chromatograph, with reference substance chromatograph relevant position on, should show the speckle of same color;
B. get embodiment 2 pharmaceutical compositions, be ground into pulpous state, get 30g, add 60-90 ℃ of petroleum ether 300ml, reflux 30 minutes filters, and reclaims solvent, and residue adds cyclohexane extraction 1ml makes dissolving, as need testing solution; Other gets Herba Pogostemonis control medicinal material 0.5g, gets control medicinal material solution with legal system; According to the test of thin chromatography, draw each 10 μ l of above-mentioned solution, put respectively in same be the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with 10: 1 60-90 ℃ petroleum ether-ethyl acetate, launch, take out, dry; Spray is with 5% anisaldehyde sulfuric acid solution, and it is clear to dry by the fire to the speckle colour developing in 110 ℃; In the test sample chromatograph, with reference substance chromatograph relevant position on, should show the speckle of same color;
C. get embodiment 2 pharmaceutical compositions, be ground into pulpous state, get 10g, add Diluted Alcohol 100ml, 350W, 50KHz supersound process 30min takes out, and puts coldly, filters, and evaporate to dryness, residue add Diluted Alcohol 5ml dissolving, as need testing solution; It is an amount of that other gets the arginine reference substance, adds Diluted Alcohol and make the solution that every 1ml contains 0.2mg, in contrast product solution; According to the test of thin chromatography, draw each 5 μ l of above-mentioned solution, put respectively in same be the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with 19: 5: 5 n-butyl alcohol-glacial acetic acid-water, launch, take out, dry; Spray is with ninhydrin solution, and it is clear to dry by the fire to the speckle colour developing in 105 ℃; In the test sample chromatograph, with reference substance chromatograph relevant position on, should show the speckle of same color;
According to high effective liquid chromatography for measuring; Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; 87: 13: 0.1 methanol-water-phosphoric acid are mobile phase; The detection wavelength is 208nm; Number of theoretical plate calculates by the oleanolic acid peak should be not less than 3000; The preparation of reference substance solution: it is an amount of that precision takes by weighing the oleanolic acid reference substance, adds methanol and make the solution that every 1ml contains 0.1mg, promptly; The preparation of need testing solution: it is an amount of to get embodiment 2 samples, is ground into pulpous state, gets about 10g, the accurate title, decide, and adds methanol 200ml, reflux 2 hours, filter, the medicinal residues methanol wash, washing liquid is incorporated filtrate into, reclaim methanol, the residue dissolve with methanol, transfer and standardize solution are to the 10ml measuring bottle, shake up, cross 0.45 μ m microporous filter membrane, get subsequent filtrate, promptly; Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
Claims (7)
1, a kind of gel for the treatment of the pharmaceutical composition of viral influenza is characterized in that the raw material of making this gel preparation consists of:
Radix Isatidis 72 weight portion Gypsum Fibrosum 32 weight portion Radix Rehmanniae 18 weight portions
Herba Pogostemonis 16 weight portion Fructus Forsythiaes 26 weight portion Rhizoma Phragmitiss 34 weight portions
The Radix Curcumae 14 weight portion Rhizoma Acori Graminei 14 weight portion Rhizoma Anemarrhenaes 14 weight portions
Sucrose 100 weight portion aspartames 1.0 weight portion citric acid 2 weight portions
Sodium alginate 11 weight portion potassium sorbate 1.0 weight portions.
2, the preparation method of pharmaceutical composition gel as claimed in claim 1 is characterized in that this method is:
Step 1: the compositions raw material of getting it filled, the Fructus Forsythiae of Radix Curcumae, Rhizoma Acori Graminei and 50% is placed in the extractor, carry most volatile oil, medicinal liquid filters, and filtrate and volatile oil are standby;
Step 2: the decocting that above residue and Radix Isatidis, Gypsum Fibrosum, Radix Rehmanniae, Rhizoma Phragmitis, the Rhizoma Anemarrhenae five tastes is added 6-10 times of weight portion boils 2-4 time, each 1-2 hour, collecting decoction, filter, filtrate and step 1 standby filtrate and volatile oil merge, being condensed into 40 ℃ of-60 ℃ of relative densities is the clear paste of 1.20-1.25, adds the dilution of 400-900 weight parts water, filters;
Step 3: the Fructus Forsythiae powder of Herba Pogostemonis and 50% is broken into fine powder, join in the above-mentioned medicinal liquid, stir evenly, other gets sucrose, aspartame, citric acid and potassium sorbate, add water to dissolving, filter, join in the above-mentioned medicinal liquid, add sodium alginate, add the water stirring and boil the gel that is 1.05-1.25 to 75-95 ℃ of following relative density.
3, pharmaceutical composition gel preparation method as claimed in claim 2 is characterized in that this method is:
Step 1: the compositions raw material of getting it filled, the Fructus Forsythiae of Radix Curcumae, Rhizoma Acori Graminei and 50% is placed in the extractor, carry most volatile oil, medicinal liquid filters, and filtrate and volatile oil are standby;
Step 2: the decocting that above residue and Radix Isatidis, Gypsum Fibrosum, Radix Rehmanniae, Rhizoma Phragmitis, the Rhizoma Anemarrhenae five tastes is added 9 times of weight portions boils 3 times, each 1.5 hours, collecting decoction, filter, filtrate and step 1 standby filtrate and volatile oil merge, the clear paste that to be condensed into 50 ℃ of relative densities be 1.20-1.25 adds the dilution of 800 weight parts waters, filters;
Step rapid 3: the Fructus Forsythiae powder of Herba Pogostemonis and 50% is broken into fine powder, join in the above-mentioned medicinal liquid, stir evenly, other gets sucrose, aspartame, citric acid and potassium sorbate, add water to dissolving, filter, join in the above-mentioned medicinal liquid, add sodium alginate, adding that water stirs and boil to 80 ℃ of following relative densities is 1.10 gel.
4, the quality determining method of pharmaceutical composition gel as claimed in claim 1 is characterized in that this method comprises following discriminating:
A. the compositions gel of getting it filled is ground into pulpous state, gets 20g, adds water 80-100ml, reflux 20-30 minute, filter, filtrate is transferred pH to 1-3 with 4-8mol/L hydrochloric acid, extracts with ether 15-25ml, reclaim ether, residue adds dehydrated alcohol 0.3-0.8ml makes dissolving, as test sample; Other evens up pier fruit acid reference substance, adds dehydrated alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to the test of thin chromatography, draw each 5 μ l of above-mentioned solution, put respectively in same be the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 8-12: 1 chloroform-methanol is developing solvent, launches, and takes out, and dries; Spray is with the 5%-15% sulfuric acid solution, and it is clear to dry by the fire to the speckle colour developing at 100 ℃-115 ℃; In the test sample chromatograph, with reference substance chromatograph relevant position on, should show the speckle of same color;
B. the compositions gel of getting it filled is ground into pulpous state, gets 30g, adds 60-90 ℃ of petroleum ether 250ml-350ml, and reflux 20-30 minute, filter, reclaim solvent, residue adds cyclohexane extraction 1ml makes dissolving, as need testing solution; Other gets Herba Pogostemonis control medicinal material 0.5g, gets control medicinal material solution with legal system; According to the test of thin chromatography, draw each 10 μ l of above-mentioned solution, put respectively in same be the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 8-12: 1 60-90 ℃ petroleum ether-ethyl acetate is developing solvent, launches, and takes out, and dries; Spray is with 5% anisaldehyde sulfuric acid solution, and it is clear to dry by the fire to the speckle colour developing in 100 ℃-120 ℃; In the test sample chromatograph, with reference substance chromatograph relevant position on, should show the speckle of same color; C. get this pharmaceutical composition, be ground into pulpous state, get 10g, add Diluted Alcohol 80ml-120ml, 350W, 50KHz supersound process 20-30min takes out, and puts coldly, filters, and evaporate to dryness, residue add Diluted Alcohol 5ml dissolving, as need testing solution; It is an amount of that other gets the arginine reference substance, adds Diluted Alcohol and make the solution that every 1ml contains 0.2mg, in contrast product solution; According to the test of thin chromatography, draw each 5 μ l of above-mentioned solution, put respectively in same be the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with 15-20: 3-7: 3-7 n-butyl alcohol-glacial acetic acid-water is developing solvent, launches, and takes out, and dries; Spray is with ninhydrin solution, and it is clear to dry by the fire to the speckle colour developing in 100 ℃-115 ℃; In the test sample chromatograph, with reference substance chromatograph relevant position on, should show the speckle of same color.
5, the quality determining method of pharmaceutical composition gel as claimed in claim 4 is characterized in that this method comprises following discriminating:
A. the compositions gel of getting it filled is ground into pulpous state, gets 20g, adds water 100ml, and reflux 30 minutes filters, and filtrate is transferred pH to 2 with 6mol/L hydrochloric acid, extracts with ether 20ml, reclaims ether, and residue adds dehydrated alcohol 0.5ml makes dissolving, as test sample; Other evens up pier fruit acid reference substance, adds dehydrated alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to the test of thin chromatography, draw each 5 μ l of above-mentioned solution, put respectively in same be the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with 10: 1 chloroform-methanols, launch, take out, dry; Spray is with 10% sulfuric acid solution, and it is clear to dry by the fire to the speckle colour developing at 105 ℃; In the test sample chromatograph, with reference substance chromatograph relevant position on, should show the speckle of same color;
B. the compositions gel of getting it filled is ground into pulpous state, gets 30g, adds 60-90 ℃ of petroleum ether 300ml, and reflux 30 minutes filters, and reclaims solvent, and residue adds cyclohexane extraction 1ml makes dissolving, as need testing solution; Other gets Herba Pogostemonis control medicinal material 0.5g, gets control medicinal material solution with legal system; According to the test of thin chromatography, draw each 10 μ l of above-mentioned solution, put respectively in same be the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with 10: 1 60-90 ℃ petroleum ether-ethyl acetate, launch, take out, dry; Spray is with 5% anisaldehyde sulfuric acid solution, and it is clear to dry by the fire to the speckle colour developing in 110 ℃; In the test sample chromatograph, with reference substance chromatograph relevant position on, should show the speckle of same color;
C. the compositions gel of getting it filled is ground into pulpous state, gets 10g, adds Diluted Alcohol 100ml, 350W, and 50KHz supersound process 30min takes out, and puts coldly, filters, and evaporate to dryness, residue add Diluted Alcohol 5ml dissolving, as need testing solution; It is an amount of that other gets the arginine reference substance, adds Diluted Alcohol and make the solution that every 1ml contains 0.2mg, in contrast product solution; According to the test of thin chromatography, draw each 5 μ l of above-mentioned solution, put respectively in same be the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with 19: 5: 5 n-butyl alcohol-glacial acetic acid-water, launch, take out, dry; Spray is with ninhydrin solution, and it is clear to dry by the fire to the speckle colour developing in 105 ℃; In the test sample chromatograph, with reference substance chromatograph relevant position on, should show the speckle of same color.
6, the quality determining method of pharmaceutical composition gel as claimed in claim 1 is characterized in that this method comprises following assay:
According to high effective liquid chromatography for measuring; Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; 80-90: 10-15: 0.1 methanol-water-phosphoric acid is a mobile phase; The detection wavelength is 208nm; Number of theoretical plate calculates by the oleanolic acid peak should be not less than 3000; The preparation of reference substance solution: it is an amount of that precision takes by weighing the oleanolic acid reference substance, adds methanol and make the solution that every 1ml contains 0.1mg, promptly; The preparation of need testing solution: sample thief is an amount of, is ground into pulpous state, gets about 10g, the accurate title, decide, and adds methanol 150ml-200ml, reflux 3-4 hour, filter, the medicinal residues methanol wash, washing liquid is incorporated filtrate into, reclaim methanol, the residue dissolve with methanol, transfer and standardize solution are to the 10ml measuring bottle, shake up, cross 0.45 μ m microporous filter membrane, get subsequent filtrate, promptly; Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
7, the quality determining method of pharmaceutical composition gel as claimed in claim 6 is characterized in that this method comprises following assay:
According to high effective liquid chromatography for measuring:
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; 87: 13: 0.1 methanol-water-phosphoric acid are mobile phase; The detection wavelength is 208nm; Number of theoretical plate calculates by the oleanolic acid peak should be not less than 3000; The preparation of reference substance solution: it is an amount of that precision takes by weighing the oleanolic acid reference substance, adds methanol and make the solution that every 1ml contains 0.1mg, promptly; The preparation of need testing solution: sample thief is an amount of, is ground into pulpous state, gets about 10g, the accurate title, decide, and adds methanol 200ml, reflux 2 hours, filter, the medicinal residues methanol wash, washing liquid is incorporated filtrate into, reclaim methanol, the residue dissolve with methanol, transfer and standardize solution are to the 10ml measuring bottle, shake up, cross 0.45 μ m microporous filter membrane, get subsequent filtrate, promptly; Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
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| CNB2006100745289A CN100453114C (en) | 2006-04-27 | 2006-04-27 | Composition of Chinese traditional medicine for treating cold in virulence, and preparation method |
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| CN112168940A (en) * | 2020-10-22 | 2021-01-05 | 佛山市高明区(中国科学院)新材料产业研究院 | Method for extracting water-soluble effective components of oral liquid for treating tetanus septicemia |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1327756A (en) * | 2001-06-01 | 2001-12-26 | 贵州大春药业有限公司 | Health-care jelly for children |
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| CN1327756A (en) * | 2001-06-01 | 2001-12-26 | 贵州大春药业有限公司 | Health-care jelly for children |
Non-Patent Citations (2)
| Title |
|---|
| 中华人民共和国卫生部颁标准中药成方制剂. 89，中华人民共和国卫生部. 1998 |
| 中华人民共和国卫生部颁标准中药成方制剂. 89，中华人民共和国卫生部. 1998 * |
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