CN100531774C - A Chinese medicinal composition for treating cough and preparation method thereof - Google Patents
A Chinese medicinal composition for treating cough and preparation method thereof Download PDFInfo
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- CN100531774C CN100531774C CNB2006100745274A CN200610074527A CN100531774C CN 100531774 C CN100531774 C CN 100531774C CN B2006100745274 A CNB2006100745274 A CN B2006100745274A CN 200610074527 A CN200610074527 A CN 200610074527A CN 100531774 C CN100531774 C CN 100531774C
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Abstract
The invention relates to a pharmaceutical composition for treating cough and process for preparation, wherein the composition is prepared from snake gall extract, fritillary, cane sugar, aspartame, citric acid, sodium alginate, potassium sorbate and pharmaceutically acceptable excipient.
Description
Technical field
The present invention relates to a kind of Chinese medicine composition and preparation method thereof and quality determining method, particularly a kind of Chinese medicine composition for the treatment of upper respiratory tract infection and preparation method thereof and quality determining method.
Background technology
Cough due to pathogenic wind-heat's symptom mainly shows as fever, xerostomia, have a stuffy nose, tell yellow sputum and ungratifying ejection of phlegm, laryngalgia.Heavy wind and heat dispersing in the treatment, it is not well to cough, and expectorant is swallowed red xerostomia based on yellow thickness, nasal obstruction stream yellow thick nasal discharge, or the heat that occurs together has antiperspirant, the profound and subtle HUANGBAI(sic) of tongue fur.Floating and rapid pulse is controlled with relieving the exterior syndrome with drugs of pungent in flavor and cool in nature, the lung qi dispersing cough-relieving.
Cough can divide heat syndrome cough and cold coughing.Recurrent cough, xerostomia, the expectorant that is caused by lung-heat is few, sticky, yellow skin, pharyngalgia or be heat syndrome cough with symptoms such as heating, headaches, should select the Fel Serpentis et Bulbus Fritillariae Cirrhosae Liquidus relieving cough and resolving phlegm for use.Because Bulbus Fritillariae Cirrhosae nature and flavor hardship, sweet, cool is gone into lung meridian, the heat clearing away eliminating stagnation is arranged, the merit of lung moistening, Fel Serpentis has heat-clearing and toxic substances removing to heighten the effect of a treatment.So Fel Serpentis et Bulbus Fritillariae Cirrhosae Liquidus truly has significant curative effect to the chronic cough of cough due to lung-heat or interior-heat caused by deficiency of YIN.
The throat that causes by catching cold itch cough frequently, sputum is thin as foamed, is to belong to cold to cough, should not take Fel Serpentis et Bulbus Fritillariae Cirrhosae Liquidus this moment, in order to avoid increase the weight of the state of an illness.
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:
Fel Serpentis 2-40 weight portion Bulbus Fritillariae Ussuriensis 50-200 weight portion sucrose 30-150 weight portion
Aspartame 0.1-2 weight portion citric acid 0.1-2 weight portion sodium alginate 1-20 weight portion
Potassium sorbate 0.1-2 weight portion.
The preferred weight proportioning of above-mentioned raw materials is as follows:
Fel Serpentis 20 weight portion Bulbus Fritillariae Ussuriensiss 150 weight portion sucrose 100 weight portions
Aspartame 1 weight portion citric acid 1 weight portion sodium alginate 10 weight portions
Potassium sorbate 1 weight portion.
The preferred weight proportioning of above-mentioned raw materials is as follows:
Fel Serpentis 4 weight portion Bulbus Fritillariae Ussuriensiss 180 weight portion sucrose 40 weight portions
Aspartame 1.9 weight portion citric acid 0.3 weight portion sodium alginate 8 weight portions
Potassium sorbate 0.2 weight portion.
The preferred weight proportioning of above-mentioned raw materials is as follows:
Fel Serpentis 38 weight portion Bulbus Fritillariae Ussuriensiss 60 weight portion sucrose 140 weight portions
Aspartame 0.2 weight portion citric acid 1.8 weight portion sodium alginates 2 weight portions
Potassium sorbate 1.7 weight portions.
Chinese medicine composition raw material of the present invention adds according to common process, makes clinical acceptable gel preparation.
The concrete preparation technology of present composition gel preparation is as follows:
The Bulbus Fritillariae Uninbracteatae of making even, add alcohol reflux 1-3 time that 8-12 doubly measures 70%-90% at every turn, each 1-3 hour, extracting solution filters, filtrate is condensed into fluid extract, add the dilution of 400-900 weight parts water, filter, other gets sucrose, aspartame, citric acid and potassium sorbate, adds water and is heated to dissolving, filter, join in the above-mentioned medicinal liquid, add sodium alginate and Fel Serpentis, aqua armeniacae, the Mentholum alcoholic solution that 0.1-1ml is saturated stirs, add water and stir and boil, the gel that to make 75-95 ℃ of following relative density be 1.05-1.25.
The preferred for preparation technology of the present composition is as follows:
The Bulbus Fritillariae Uninbracteatae of making even adds the alcohol reflux 2 times of 10 times of amounts 80%, each 2 hours at every turn, extracting solution filters, and filtrate is condensed into fluid extract, adds the dilution of 800 weight parts waters, filter, other gets sucrose, aspartame, citric acid and potassium sorbate, adds water and is heated to dissolving, filter, join in the above-mentioned medicinal liquid, add sodium alginate and Fel Serpentis, aqua armeniacae, the Mentholum alcoholic solution that 0.5ml is saturated stirs, add water and stir and boil, make 80 ℃ of following relative densities and be 1.10 gel.
Quality determining method of the present invention comprises following discrimination method and/or content assaying method
Discrimination method comprises one or more in the following discriminating:
A. get pharmaceutical composition gel 40g of the present invention, be ground into pulpous state, add strong aqua ammonia 10ml, chloroform 30ml, 350W, 50KHz supersound process 30 minutes, put cold, filter, it is standby to get chloroform solution, and the strong aqua ammonia layer extracts 3 times with the water-saturated n-butanol jolting, 20ml for the first time, 20ml for the second time, 10ml for the third time, jolting is extracted, merge n-butanol extracting liquid, wash with water 2 times, for the first time 20ml, 15ml for the second time, divide and get n-butyl alcohol liquid, put evaporate to dryness in the water-bath, residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution; It is an amount of that other gets Fel Serpentis, adds ethanol and make the solution that every 1ml contains 5mg, in contrast medical material solution; It is an amount of to get the sodium taurocholate reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 2 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with sodium carboxymethyl cellulose, with 10:1:1 n-butyl alcohol-glacial acetic acid-water is developing solvent, launches, and takes out, dry, spray is with 30% ethanol solution of sulfuric acid, and it is clear to dry by the fire to the speckle colour developing at 105 ℃, puts under the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
B. the compositions gel 40g that gets it filled is ground into pulpous state, adds strong aqua ammonia 10ml, chloroform 30ml, and 350W, 50KHz supersound process 30 minutes is put coldly, filters, and gets chloroform solution, puts evaporate to dryness in the water-bath, and residue adds dehydrated alcohol 0.5ml makes dissolving, as need testing solution; Other is the Bulbus Fritillariae Uninbracteatae control medicinal material 2g that makes even, with 80% alcohol heating reflux 2 hours, filter, filtrate is put and is moved into separatory funnel when steaming to 2ml in the water-bath, transfers to alkalescence with strong ammonia solution, and 20ml divides second extraction with chloroform, the combined chloroform layer, put evaporate to dryness in the water-bath, residue adds dehydrated alcohol 0.5ml makes dissolving, in contrast medical material solution; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with sodium carboxymethyl cellulose, with 12:2:1 ethyl acetate-methanol-strong ammonia solution is developing solvent, launches, and takes out, dry, spray successively with rare bismuth potassium iodide test solution and sodium nitrite ethanol test solution, placed 1 minute, observe; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Content assaying method in the quality determining method is as follows:
Precision is measured pharmaceutical composition gel 75g of the present invention, is ground into pulpous state, puts in the 500ml kjeldahl flask, adds water 200ml, connects condensing tube, water flowing steam distillation, and distillate imports in 10ml, the 90% alcoholic acid absorption liquid, and receiving bottle is put in the ice bath and is cooled off; Stop distillation when the distillate full dose reaches 150ml, add each 2ml of potassium iodide test solution and ammonia solution in distillate, with the slowly titration of 0.005mol/L silver nitrate solution, the yellow-white muddiness of showing to solution does not disappear, and titration results is proofreaied and correct with blank assay, promptly; Every 1ml silver nitrate solution (0.005mol/L) is equivalent to the HCN of 0.27025mg.
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.The shake bile-fritillary preparation is mainly used in the treatment cough due to pathogenic wind-heat, abundant expectoration asthma, and uncomfortable in chest, expectoration is not well or chronic cough is more than.At present, existing listing have only the shake bile-fritillary oral liquid because main component all is dissolved in the solution, the taste of some composition is difficult to cover, and makes the child be unwilling to take.We have made the fruit jelly gel that liked by the child on the basis of original prescription, good in mouthfeel when the patient takes because active component in gel-type vehicle, has been covered disagreeable taste, taste is suitable, 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 experimentation of experimental example 1 Bulbus Fritillariae Ussuriensis alcohol extraction process conditions
1, trial test
Take by weighing Bulbus Fritillariae Ussuriensis 150g, add the alcohol reflux secondary of 10 times of amounts 80%, each 2 hours, extracting solution filtered, filtrate recycling ethanol, and water-bath is steamed near and is done, vacuum drying (70 ℃-0.09Mpa), about 22.5g gets dry extract.
2, orthogonal test: because clearly do not add alcohol doubly amount, backflow number of times, return time in the quality standard of Fel Serpentis et Bulbus Fritillariae Cirrhosae Liquidus, so we with add alcohol doubly amount, backflow number of times, return time be that the screening factor is selected, use L
9(3
4) orthogonal table carries out orthogonal test and carry out orthogonal test, as controlling index, carries out process optimization with the total amount of total alkaloids in the dried cream.Factor, level see Table 1:
Table 1 alcohol extraction orthogonal test factor level table
Operational approach: take by weighing Bulbus Fritillariae Ussuriensis 150g at every turn, add 80% alcohol reflux, extracting solution filters, filtrate recycling ethanol, and water-bath is steamed near and is done, (70 ℃-0.09Mpa), get dry extract and weigh and measure total alkaloid contents of vacuum dryings.The results are shown in Table 2:
Table 2 orthogonal array and index determining result
Table 3 variance of totals analytical table
F
1-0.1(2，2)＝99；F
1-0.05(2，2)＝19；F
1-0.10(2，2)＝9
Above-mentioned test shows that the A factor promptly adds alcohol and doubly measures variant F
1-0.10(2,2)＜F＜F
1-0.05(2,2), average 2 and average 3 difference are considered and are economized on alcohol, so select A not quite and all obviously greater than average 1
2The B factor number of times that promptly refluxes has significant difference, F
1-0.05(2,2)＜F＜F
1-0.01The saving cost is considered, so select B not quite and all obviously greater than average 1 in (2,2), average 2 and average 3 difference
2The C factor is the variant F of return time
1-0.10(2,2)＜F＜F
1-0.05(2,2), from average, average 2 and average 3 difference are not quite and all obviously greater than average 1, in order to save time, so select C
2Therefore, comprehensive various factors considers that extraction process is defined as A
2B
2C
2, promptly add 10 times at every turn and measure 80% alcohol reflux secondary, each 2 hours.
3, demonstration test: the Bulbus Fritillariae Uninbracteatae 150g that makes even adds 10 times at every turn and measures 80% alcohol reflux secondary, each 2 hours, extracting solution filters, filtrate recycling ethanol, and water-bath is steamed near and is done, (70 ℃-0.09Mpa), get dry extract and weigh and measure total alkaloid contents of vacuum dryings.Test parallel carrying out three times, the result is as follows:
Table 4 checking result
By above result as can be seen, three result of the test opposing parallel have repeatability preferably, and this feasible process is described.
Experimental example 2 prescription screening research experiments
1, definite experiment of sodium alginate amount and citric acid amount
Do the preliminary preparation of gel, with the amount of definite sodium alginate and the amount of citric acid, Bulbus Fritillariae Uninbracteatae fluid extract 7.5ml, Fel Serpentis 1g, aqua armeniacae 3ml make even at every turn, add 40ml water, stir, filter, add 10g Icing Sugar, 0.1g potassium sorbate, after the stirring, add the citric acid and the sodium alginate of different proportion at last, add water to 55g, 80-90 ℃ of insulations are also stirred 40-60min, take out, cool off under the room temperature, promptly.Observe the character and the taste of gel.
The addition test of table 5 sodium alginate
Conclusion: prescription 1 does not add citric acid, and the gel color is dark as a result, gel is soft slightly, taste is poor than other prescription.Prescription 2, prescription 3 and write out a prescription 4 relatively, 3 gels of writing out a prescription are neither too hard, nor too soft, and mouthfeel is better, determines that therefore the addition of citric acid is 0.1%, and the addition of sodium alginate is 1.0%.
2, the screening experiment of sweeting agent and consumption thereof
It is Bulbus Fritillariae Ussuriensis fluid extract 7.5ml, Fel Serpentis 1g, aqua armeniacae 3ml that 10 bags of amounts are got in each test, add the suitable quantity of water dilution, filter, add Icing Sugar, aspartame according to following table, mouth gustation road, choose the good person of taste and add sodium alginate and potassium sorbate, add water to 55g, 80-90 ℃ of insulations also add a small amount of Mentholum, stir 40-50min simultaneously, take out, cool off under the room temperature, observe the character and the taste of gel.
Table 6 prescription screening table
Conclusion: 1,2, No. 3 short sweetness are bitter slightly.No. 5 sweet excessively, and No. 4 mouthfeel is better, and sugariness is moderate, and little hardship is so finally select No. 4 prescriptions to be this product preparation prescription.Mentholum is volatile, so should add Mentholum after 80-90 ℃ of insulation, stirs evenly.
Consider in the production that sucrose needn't be ground into fine powder, but impurity is arranged, need to add the suitable quantity of water heating for dissolving, filter the back and use.Gel is in order to reach the effect of sterilization in addition, and gel boils 80-90 ℃ of insulation in back and fill, and the preparing gel process summary is as follows:
Get fluid extract, add the suitable quantity of water dilution, filter, other gets 10% sucrose, 0.1% aspartame, 0.1% citric acid and 0.1% potassium sorbate, adds the suitable quantity of water heating for dissolving, filters, join in the above-mentioned medicinal liquid, add 1.0% sodium alginate and Fel Serpentis, aqua armeniacae, stir, add water to ormal weight, stir and boil, in 80-90 ℃ of insulation and add a small amount of Mentholum, stir evenly, fill, every packed 5g, promptly.
The experiment of experimental example 3 technology repeatability
Take by weighing medical material by formulate prescription, every batch in 1000g, prepares three batches altogether:
Prescription:
Fel Serpentis 20g Bulbus Fritillariae Ussuriensis 150g
Method for making: above two flavors, the Bulbus Fritillariae Uninbracteatae of making even adds twice of 10 times of amount 80% alcohol reflux at every turn, each 2 hours, merge extractive liquid, filtered, decompression filtrate recycling ethanol and concentrating under reduced pressure become fluid extract, add the suitable quantity of water dilution, filter, other gets 10% sucrose, 0.1% aspartame, 0.1% citric acid and 0.1% potassium sorbate, add the suitable quantity of water heating for dissolving, filter, join in the above-mentioned medicinal liquid, add 1.0% sodium alginate and Fel Serpentis, aqua armeniacae 60ml, stir, add water to ormal weight, stir and boil, in 80-90 ℃ of insulation, adding a small amount of Mentholum stirs evenly, fill, every packed 5g, promptly.The result is as follows:
Table 7, technology repeatability experimental result table (1000g, 200 bags)
The result of three batches of tests shows, this technology favorable reproducibility, and process stabilizing is reliable, can carry out pilot scale research.
Experimental example 4 mandelonitrile assay experimentatioies
1, replica test
Get this product with the about 75g of a collection of shake bile-fritillary gel (050127), precision takes by weighing in right amount (5 parts), measures according to content assaying method, the results are shown in Table 8.
Table 8 replica test result
The result shows that the repeatability of this method is good.
2, sample determination is got the about 75g of this product, and accurate the title decides, and measures according to content assaying method, and 10 batch sample assays the results are shown in Table 9.
Table 9 sample determination result
Conclusion: tentative this product contains mandelonitrile in hydrocyanic acid for every bag, should be 0.1-0.3mg.
Following embodiment all can realize the effect of above-mentioned experimental example.
The specific embodiment:
Embodiment 1: the preparation of gel
Fel Serpentis 20kg Bulbus Fritillariae Ussuriensis 150kg sucrose 100kg
Aspartame 1kg citric acid 1kg sodium alginate 10kg
Potassium sorbate 1kg
The Bulbus Fritillariae Uninbracteatae of making even adds the alcohol reflux 2 times of 10 times of amounts 80%, each 2 hours at every turn, extracting solution filters, and filtrate is condensed into fluid extract, adds the dilution of 800kg water, filter, other gets sucrose, aspartame, citric acid and potassium sorbate, adds water and is heated to dissolving, filter, join in the above-mentioned medicinal liquid, add sodium alginate and Fel Serpentis, aqua armeniacae, the Mentholum alcoholic solution that 0.5ml is saturated stirs, add water and stir and boil, make 80 ℃ of following relative densities and be 1.10 gel.
Embodiment 2: the preparation of gel
Fel Serpentis 4kg Bulbus Fritillariae Ussuriensis 180kg sucrose 40kg
Aspartame 1.9kg citric acid 0.3kg sodium alginate 8kg
Potassium sorbate 0.2kg
The Bulbus Fritillariae Uninbracteatae of making even adds the alcohol reflux 3 times of 12 times of amounts 70%, each 3 hours at every turn, extracting solution filters, and filtrate is condensed into fluid extract, adds the dilution of 400kg water, filter, other gets sucrose, aspartame, citric acid and potassium sorbate, adds water and is heated to dissolving, filter, join in the above-mentioned medicinal liquid, add sodium alginate and Fel Serpentis, aqua armeniacae, the Mentholum alcoholic solution that 0.5ml is saturated stirs, add water and stir and boil, make 95 ℃ of following relative densities and be 1.05 gel.
Embodiment 3: the preparation of gel
Fel Serpentis 38kg Bulbus Fritillariae Ussuriensis 60kg sucrose 140kg
Aspartame 0.2kg citric acid 1.8kg sodium alginate 2kg
Potassium sorbate 1.7kg
The Bulbus Fritillariae Uninbracteatae of making even adds the alcohol reflux 2 times of 8 times of amounts 90%, each 2 hours at every turn, extracting solution filters, and filtrate is condensed into fluid extract, adds the dilution of 800kg water, filter, other gets sucrose, aspartame, citric acid and potassium sorbate, adds water and is heated to dissolving, filter, join in the above-mentioned medicinal liquid, add sodium alginate and Fel Serpentis, aqua armeniacae, the Mentholum alcoholic solution that 0.2ml is saturated stirs, add water and stir and boil, make 75 ℃ of following relative densities and be 1.15 gel.
Embodiment 4: the preparation of gel
Fel Serpentis 10kg Bulbus Fritillariae Ussuriensis 160kg sucrose 50kg
Aspartame 1.6kg citric acid 0.5kg sodium alginate 17kg
Potassium sorbate 0.6kg
The Bulbus Fritillariae Uninbracteatae of making even adds the alcohol reflux 2 times of 10 times of amounts 80%, each 3 hours at every turn, extracting solution filters, and filtrate is condensed into fluid extract, adds the dilution of 700kg water, filter, other gets sucrose, aspartame, citric acid and potassium sorbate, adds water and is heated to dissolving, filter, join in the above-mentioned medicinal liquid, add sodium alginate and Fel Serpentis, aqua armeniacae, the Mentholum alcoholic solution that 0.2ml is saturated stirs, add water and stir and boil, make 85 ℃ of following relative densities and be 1.10 gel.
Embodiment 5: the preparation of gel
Fel Serpentis 30kg Bulbus Fritillariae Ussuriensis 70kg sucrose 120kg
Aspartame 0.8kg citric acid 1.7kg sodium alginate 6kg
Potassium sorbate 1.5kg
The Bulbus Fritillariae Uninbracteatae of making even adds the alcohol reflux 3 times of 12 times of amounts 90%, each 3 hours at every turn, extracting solution filters, and filtrate is condensed into fluid extract, adds the dilution of 900kg water, filter, other gets sucrose, aspartame, citric acid and potassium sorbate, adds water and is heated to dissolving, filter, join in the above-mentioned medicinal liquid, add sodium alginate and Fel Serpentis, aqua armeniacae, the Mentholum alcoholic solution that 0.4ml is saturated stirs, add water and stir and boil, make 90 ℃ of following relative densities and be 1.10 gel.
Embodiment 6: the discrimination method in the quality testing
A. get the gel 40g of embodiment 1, be ground into pulpous state, add strong aqua ammonia 10ml, chloroform 30ml, 350W, 50KHz supersound process 30 minutes is put coldly, filters, it is standby to get chloroform solution, and the strong aqua ammonia layer extracts 3 times with the water-saturated n-butanol jolting, for the first time 20ml, 20ml for the second time, 10ml for the third time, jolting is extracted, and merges n-butanol extracting liquid, washes with water 2 times, 20ml for the first time, 15ml divides and gets n-butyl alcohol liquid for the second time, put evaporate to dryness in the water-bath, residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution; It is an amount of that other gets Fel Serpentis, adds ethanol and make the solution that every 1ml contains 5mg, in contrast medical material solution; It is an amount of to get the sodium taurocholate reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 2 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with sodium carboxymethyl cellulose, with 10:1:1 n-butyl alcohol-glacial acetic acid-water is developing solvent, launches, and takes out, dry, spray is with 30% ethanol solution of sulfuric acid, and it is clear to dry by the fire to the speckle colour developing at 105 ℃, puts under the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
B. get the chloroform layer of a Fel Serpentis discriminating following need testing solution among the A, put evaporate to dryness in the water-bath, residue adds dehydrated alcohol 0.5ml makes dissolving, as need testing solution; Other is the Bulbus Fritillariae Uninbracteatae control medicinal material 2g that makes even, with 80% alcohol heating reflux 2 hours, filter, filtrate is put and is moved into separatory funnel when steaming to 2ml in the water-bath, transfers to alkalescence with strong ammonia solution, and 20ml divides second extraction with chloroform, the combined chloroform layer, put evaporate to dryness in the water-bath, residue adds dehydrated alcohol 0.5ml makes dissolving, in contrast medical material solution; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with sodium carboxymethyl cellulose, with 12:2:1 ethyl acetate-methanol-strong ammonia solution is developing solvent, launches, and takes out, dry, spray successively with rare bismuth potassium iodide test solution and sodium nitrite ethanol test solution, placed 1 minute, observe; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Embodiment 7: the content assaying method in the quality testing
Precision is measured the gel 75g of embodiment 2, is ground into pulpous state, puts in the 500ml kjeldahl flask, adds water 200ml, connects condensing tube, water flowing steam distillation, and distillate imports in 10ml, the 90% alcoholic acid absorption liquid, and receiving bottle is put in the ice bath and is cooled off; Stop distillation when the distillate full dose reaches 150ml, add each 2ml of potassium iodide test solution and ammonia solution in distillate, with the slowly titration of 0.005mol/L silver nitrate solution, the yellow-white muddiness of showing to solution does not disappear, and titration results is proofreaied and correct with blank assay, promptly; Every 1ml silver nitrate solution (0.005mol/L) is equivalent to the HCN of 0.27025mg.
Embodiment 8: quality monitoring method
A. get the gel 40g of embodiment 3, be ground into pulpous state, add strong aqua ammonia 10ml, chloroform 30ml, 350W, 50KHz supersound process 30 minutes is put coldly, filters, it is standby to get chloroform solution, and the strong aqua ammonia layer extracts 3 times with the water-saturated n-butanol jolting, for the first time 20ml, 20ml for the second time, 10ml for the third time, jolting is extracted, and merges n-butanol extracting liquid, washes with water 2 times, 20ml for the first time, 15ml divides and gets n-butyl alcohol liquid for the second time, put evaporate to dryness in the water-bath, residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution; It is an amount of that other gets Fel Serpentis, adds ethanol and make the solution that every 1ml contains 5mg, in contrast medical material solution; It is an amount of to get the sodium taurocholate reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 2 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with sodium carboxymethyl cellulose, with 10:1:1 n-butyl alcohol-glacial acetic acid-water is developing solvent, launches, and takes out, dry, spray is with 30% ethanol solution of sulfuric acid, and it is clear to dry by the fire to the speckle colour developing at 105 ℃, puts under the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
B. get the chloroform layer of a Fel Serpentis discriminating following need testing solution among the A, put evaporate to dryness in the water-bath, residue adds dehydrated alcohol 0.5ml makes dissolving, as need testing solution; Other is the Bulbus Fritillariae Uninbracteatae control medicinal material 2g that makes even, with 80% alcohol heating reflux 2 hours, filter, filtrate is put and is moved into separatory funnel when steaming to 2ml in the water-bath, transfers to alkalescence with strong ammonia solution, and 20ml divides second extraction with chloroform, the combined chloroform layer, put evaporate to dryness in the water-bath, residue adds dehydrated alcohol 0.5ml makes dissolving, in contrast medical material solution; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with sodium carboxymethyl cellulose, with 12:2:1 ethyl acetate-methanol-strong ammonia solution is developing solvent, launches, and takes out, dry, spray successively with rare bismuth potassium iodide test solution and sodium nitrite ethanol test solution, placed 1 minute, observe; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
Precision is measured the gel 75g of embodiment 3, is ground into pulpous state, puts in the 500ml kjeldahl flask, adds water 200ml, connects condensing tube, water flowing steam distillation, and distillate imports in 10ml, the 90% alcoholic acid absorption liquid, and receiving bottle is put in the ice bath and is cooled off; Stop distillation when the distillate full dose reaches 150ml, add each 2ml of potassium iodide test solution and ammonia solution in distillate, with the slowly titration of 0.005mol/L silver nitrate solution, the yellow-white muddiness of showing to solution does not disappear, and titration results is proofreaied and correct with blank assay, promptly; Every 1ml silver nitrate solution (0.005mol/L) is equivalent to the HCN of 0.27025mg.
Claims (4)
1, a kind of pharmaceutical composition gel preparation for the treatment of cough is characterized in that this gel preparation made by following method:
Fel Serpentis 20kg Bulbus Fritillariae Ussuriensis 150kg sucrose 100kg
Aspartame 1kg citric acid 1kg sodium alginate 10kg
Potassium sorbate 1kg;
The Bulbus Fritillariae Uninbracteatae of making even adds the alcohol reflux 2 times of 10 times of amounts 80%, each 2 hours at every turn, extracting solution filters, and filtrate is condensed into fluid extract, adds the dilution of 800kg water, filter, other gets sucrose, aspartame, citric acid and potassium sorbate, adds water and is heated to dissolving, filter, join in the above-mentioned medicinal liquid, add sodium alginate and Fel Serpentis, aqua armeniacae 60L, the Mentholum alcoholic solution that 0.5ml is saturated stirs, add water and stir and boil, make 80 ℃ of following relative densities and be 1.10 gel.
2, a kind of preparation method for the treatment of the pharmaceutical composition gel preparation of cough is characterized in that this method is:
Fel Serpentis 20kg Bulbus Fritillariae Ussuriensis 150kg sucrose 100kg
Aspartame 1kg citric acid 1kg sodium alginate 10kg
Potassium sorbate 1kg;
The Bulbus Fritillariae Uninbracteatae of making even adds the alcohol reflux 2 times of 10 times of amounts 80%, each 2 hours at every turn, extracting solution filters, and filtrate is condensed into fluid extract, adds the dilution of 800kg water, filter, other gets sucrose, aspartame, citric acid and potassium sorbate, adds water and is heated to dissolving, filter, join in the above-mentioned medicinal liquid, add sodium alginate and Fel Serpentis, aqua armeniacae 601, the Mentholum alcoholic solution that 0.5ml is saturated stirs, add water and stir and boil, make 80 ℃ of following relative densities and be 1.10 gel.
3, the detection method of pharmaceutical composition gel preparation as claimed in claim 1 is characterized in that this method comprises following discriminating:
A. the compositions gel 40g that gets it filled is ground into pulpous state, adds strong aqua ammonia 10ml, chloroform 30ml, 350W, 50KHz supersound process 30 minutes is put coldly, filters, it is standby to get chloroform solution, and the strong aqua ammonia layer extracts 3 times with the water-saturated n-butanol jolting, for the first time 20ml, 20ml for the second time, 10ml for the third time, jolting is extracted, and merges n-butanol extracting liquid, washes with water 2 times, 20ml for the first time, 15ml divides and gets n-butyl alcohol liquid for the second time, put evaporate to dryness in the water-bath, residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution; It is an amount of that other gets Fel Serpentis, adds ethanol and make the solution that every 1ml contains 5mg, in contrast medical material solution; It is an amount of to get the sodium taurocholate reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 2 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with sodium carboxymethyl cellulose, with 10:1:1 n-butyl alcohol-glacial acetic acid-water is developing solvent, launches, and takes out, dry, spray is with 30% ethanol solution of sulfuric acid, and it is clear to dry by the fire to the speckle colour developing at 105 ℃, puts under the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
B. the compositions gel 40g that gets it filled is ground into pulpous state, adds strong aqua ammonia 10ml, chloroform 30ml, and 350W, 50KHz supersound process 30 minutes is put coldly, filters, and gets chloroform solution, puts evaporate to dryness in the water-bath, and residue adds dehydrated alcohol 0.5ml makes dissolving, as need testing solution; Other is the Bulbus Fritillariae Uninbracteatae control medicinal material 2g that makes even, with 80% alcohol heating reflux 2 hours, filter, filtrate is put and is moved into separatory funnel when steaming to 2ml in the water-bath, transfers to alkalescence with strong ammonia solution, and 20ml divides second extraction with chloroform, the combined chloroform layer, put evaporate to dryness in the water-bath, residue adds dehydrated alcohol 0.5ml makes dissolving, in contrast medical material solution; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with sodium carboxymethyl cellulose, with 12:2:1 ethyl acetate-methanol-strong ammonia solution is developing solvent, launches, and takes out, dry, spray successively with rare bismuth potassium iodide test solution and sodium nitrite ethanol test solution, placed 1 minute, observe; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
4, the detection method of pharmaceutical composition gel preparation as claimed in claim 1 is characterized in that this method comprises following assay:
The compositions gel 75g that gets it filled is ground into pulpous state, puts in the 500ml kjeldahl flask, adds water 200ml, connects condensing tube, water flowing steam distillation, and distillate imports in 10ml, the 90% alcoholic acid absorption liquid, and receiving bottle is put in the ice bath and is cooled off; Stop distillation when the distillate full dose reaches 150ml, add each 2ml of potassium iodide test solution and ammonia solution in distillate, with the slowly titration of 0.005mol/L silver nitrate solution, the yellow-white muddiness of showing to solution does not disappear, and titration results is proofreaied and correct with blank assay, promptly; The 0.005mol/L silver nitrate solution of every 1ml is equivalent to the HCN of 0.27025mg.
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| CN104644995A (en) * | 2014-11-13 | 2015-05-27 | 新疆昌吉康隆生物科技有限公司 | Production process of sinkiang fritillary bulb fluid extract |
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| 中华人民共和国卫生部药品标准中药成方制剂第9册. 中华人民共和国卫生部药典委员会，178页. 1994 中华人民共和国药典2005年版第一部. 143，化学工业出版社. 2005 |
| 中华人民共和国卫生部药品标准中药成方制剂第9册. 中华人民共和国卫生部药典委员会，178页. 1994 * |
| 中华人民共和国药典2005年版第一部. 143，化学工业出版社. 2005 * |
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