CN101491634B - Traditional Chinese medicine composition for treating chronic pharyngitis and preparation method and quality control method thereof - Google Patents
Traditional Chinese medicine composition for treating chronic pharyngitis and preparation method and quality control method thereof Download PDFInfo
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Abstract
The invention relates to a pharmaceutical composition for treating chronic pharyngitis, in particular to a traditional Chinese medicinal composition for treating chronic pharyngitis, as well as a preparation method and a quality control method thereof. The pharmaceutical composition comprises figwort roots, radix asteris, radix asparagi, cortex moutan radicis, ophiopogon roots and other raw medicinal materials, and is prepared into various preparations suitable for clinical application according to traditional Chinese medicinal routine techniques, including tablets, capsules, orally taken liquid preparations, dropping pills, granules, and the like. The quality control method comprises qualitative identification for thin-layer chromatography, content determination of high performance liquid chromatography and other methods. The pharmaceutical composition has good effects of treating throat dryness, throat itch, irritable cough and other symptoms caused by chronic pharyngitis.
Description
Technical field
The present invention relates to a kind of pharmaceutical composition for the treatment of chronic pharyngitis, particularly a kind of Chinese medicine composition for the treatment of chronic pharyngitis and preparation method thereof and method of quality control belong to technical field of Chinese medicines.
Background technology
Chronic pharyngitis is a kind of commonly encountered diseases, for the pharyngeal pathological changes of the caused diffusivity of chronic infection, mainly is the pharyngeal mucosa inflammation.Be mainly in the adult, becoming impatient property pharyngitis, long-term dust or harmful gas stimulate its main diseases because of having repeatly, tobacco and wine excessively or other bad life habits, the stimulation of sinusitis secretions, allergic constitution or passive protective physical fitness attenuating etc.Chronic pharyngitis also can be the topical manifestations of some systemic disease, as anemia, diabetes, liver cirrhosis and chronic nephritis etc.Sickness rate accounts for about 10% to 20% of laryngopharyngeal diseases in the urbanite.Because of its course of disease is long, the symptom stubbornness, the short-term difficulty is seen produce effects, so be difficult for curing.
Chronic pharyngitis does not generally need to use antibiotic therapy, because chronic pharyngitis and non-bacterial infection.Doctor trained in Western medicine is generally paid attention to local application, as: the rinse medicine, use 2% boric acid solution, 3% saline and 1: 5000 furacilin solution be rinse repeatedly, perhaps use 2% iodine glycerol, 5% protargol liquid way in pharynx wall, or be contained in the oral cavity etc., the function of certain relief of symptoms is arranged with tabellae iodi gurgitis, oradol, Herba Menthae etc., but general being difficult to cured, and curative effect is relatively poor.
The Chinese traditional treatment primary disease focuses on and effects a permanent cure, and presses the medication of medicine typing method, and curative effect is better." element is asked the negative and positive another matter " cloud: " sore throat of monoyin and monoyang knot meaning." be argumentation the earliest to primary disease.Ancient Chinese medicine doctor has more performance, and the etiology and pathogenesis of sore throat has been done discussion from different aspects, reduces expectorant heat, asthenic fire, body fluid cannot flow upwards etc.Common drug has LIYANLING PIAN, moistening and cleaning throat Ganlu pill, Armeniaca mume Sieb. ball, sore-throat relieving tea and some buccal tablets, also has the Chinese medical spray therapy, all effect is better, so further bring into play the advantage of Chinese medicine primary disease, provides the better Chinese medicine composition of a kind of therapeutic effect to be very important.
Summary of the invention
The object of the present invention is to provide a kind of Chinese medicine composition that is used for the treatment of chronic pharyngitis;
Another object of the present invention is to provide the preparation method of this Chinese medicine composition;
The 3rd purpose of the present invention provides the method for quality control of this Chinese medicine composition.
The bright purpose of this law is achieved through the following technical solutions:
The Chinese medicine composition of treatment chronic pharyngitis of the present invention is made up of following weight portion crude drug:
Radix Scrophulariae 150～180 weight portion Radix Asteriss 120～150 weight portion Radix Asparagis 100～130 weight portions
Radix Arnebiae (Radix Lithospermi) 40～70 weight portion 50～80 weight portion Flos Farfaraees (system) Radix Ophiopogonis 40～70 weight portions
Semen Oroxyli 50～80 weight portion Radix Rehmanniae 50～80 weight portion Flos Loniceraes 200～230 weight portions
Rhizoma Belamcandae 120～150 weight portion Fructus Arctiis 40～70 weight portion Oleum menthae 0.4～0.6 weight portion
The Chinese medicine composition of treatment chronic pharyngitis of the present invention, preferred following weight portion crude drug is formed:
Radix Scrophulariae 170 weight portion Radix Asteriss 130 weight portion Radix Asparagis 120 weight portions
Radix Arnebiae (Radix Lithospermi) 50 weight portion 70 weight portion Flos Farfaraees (system) Radix Ophiopogonis 60 weight portions
Semen Oroxyli 70 weight portion Radix Rehmanniae 70 weight portion Flos Loniceraes 210 weight portions
Rhizoma Belamcandae 140 weight portion Fructus Arctiis 50 weight portion Oleum menthae 0.5 weight portion
The Chinese medicine composition of treatment chronic pharyngitis of the present invention, can also form by preferred following weight portion crude drug:
The Radix Scrophulariae 170 weight portion Radixs Stemonae (system) 130 weight portion Radix Asparagis 120 weight portions
Cortex Moutan 50 weight portion 70 weight portion Flos Farfaraees (system) Radix Ophiopogonis 60 weight portions
Semen Oroxyli 70 weight portion Radix Rehmanniae 70 weight portion Radix Isatidis 210 weight portions
Fructus Canarii 140 weight portion Periostracum Cicadaes 50 weight portion Oleum menthae 0.5 weight portion
Chinese medicine composition of the present invention is with yin nourishing, lung moistening is puted forth effort, and get heat-clearing and toxic substances removing, clearing throat, wind-dispelling heat-dissipating, relieving cough and reducing sputum, the merit that sore-throat relieving is antipruritic, to the plain body deficiency of YIN, experience the heresy of wind heat, easily the disease from dryization is very suitable, should control pharyngitis due to the acute and chronic pharyngitis, dry pharynx, itching throat, xerostomia, thirsty, cough, heating, aversion to wind, sweating and irritable cough, hoarseness, diseases such as aphonia.
Chinese medicine composition of the present invention, technology adding adjuvant is made clinical acceptable forms such as tablet, capsule, oral liquid, drop pill, granule routinely; Described adjuvant comprises solvent, disintegrating agent, correctives, antiseptic, coloring agent, binding agent, lubricant, substrate etc.
The preparation method of Chinese medicine composition tablet of the present invention is:
More than 12 the flavor, except that Oleum menthae, Flos Farfarae is crushed to 100 orders, sieves; Ten flavors such as all the other Radix Scrophulariaes decoct with water 1～3 time, and each 2～4 hours, collecting decoction, left standstill 20～30 hours, and got supernatant, being condensed into relative density is the thick paste of 1.35 (60-70 ℃), mix with Common Coltsfoot Flower,, be crushed to 80 orders at drying under reduced pressure below 60 ℃, add the sucrose of medicated powder weight 8%, make granule, spray is with Oleum menthae, the magnesium stearate that adds particle weight 0.5%, mixing is pressed into 1000, sugar coating, promptly.
The method of quality control of Chinese medicine composition of the present invention comprises one or more in following qualitative checking method and/or the quantitative detecting method:
(1) qualitative detection of Flos Farfarae
Get pharmaceutical preparation content of the present invention, adding diethyl ether makes dissolving, and supersound process is filtered, and filtrate is waved to 1.5ml, as need testing solution.
The Flos Farfarae of withdrawing the money control medicinal material is made control medicinal material solution.
According to thin layer chromatography test, draw above-mentioned two kinds of solution, respectively with same silica gel g thin-layer plate on, with developing solvent, launch, take out, dry, spray is with vanillin concentrated sulphuric acid test solution, hot blast blow develop the color to speckle clear.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(2) qualitative detection of Semen Oroxyli
Get pharmaceutical preparation content of the present invention, add the dehydrated alcohol supersound process, filter, the filtrate evaporate to dryness adds anhydrous alcohol solution as test sample.
Get the Semen Oroxyli control medicinal material, make control medicinal material solution.
According to thin layer chromatography test, draw above-mentioned sample solution, control medicinal material solution, respectively with same silica gel g thin-layer plate on, with developing solvent, launch, take out, dry, spray is with the vanillin sulfuric acid solution, hot blast blow develop the color to speckle clear.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(3) qualitative detection of Radix Ophiopogonis
Get pharmaceutical preparation content of the present invention, add the chloroform-methanol mixed liquid dipping, supersound process is filtered, and evaporate to dryness is with the chloroform dissolving, as need testing solution.
Get control medicinal material Radix Ophiopogonis, shred, make control medicinal material solution.
According to thin layer chromatography test, draw above-mentioned solution, respectively with same silica gel g thin-layer plate on, with developing solvent, launch, take out, dry, spray is with ethanol solution of sulfuric acid, hot blast blow develop the color to speckle clear.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(4) detection by quantitative of n-butyl alcohol extractum:
Get pharmaceutical preparation content of the present invention, the accurate title, decide, and the accurate methanol that adds claims to decide weight, put reflux in the water-bath, put coldly, supply the weight that subtracts mistake, filter with methanol, get subsequent filtrate, put in the evaporating dish that is dried to constant weight, evaporate to dryness, residue add water makes dissolving, use water saturated n-butanol extraction, merge n-butyl alcohol liquid, put in the evaporating dish that is dried to constant weight evaporate to dryness, 105 ℃ of dryings, in the dislocation exsiccator, place, weight decided in accurate rapidly title, calculates, promptly.
(5) detection by quantitative of harpagoside:
According to high effective liquid chromatography for measuring.
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With the acetonitrile is mobile phase A, is Mobile phase B with 1% acetum, carries out gradient elution; The detection wavelength is 278nm.Number of theoretical plate calculates by the harpagoside peak should be not less than 5000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the harpagoside reference substance, adds methanol and make reference substance solution, promptly.
Chinese medicine composition content of the present invention is got in the preparation of need testing solution, gets about 1.0g, and accurate the title decides, put in the tool plug conical flask accurate 30% methanol, the close plug of adding, claim to decide weight, after the immersion, supersound process, put coldly, claim again to decide weight, supply the weight that subtracts mistake with 30% methanol, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly.
(6) detection by quantitative of catalpol:
According to high effective liquid chromatography for measuring.
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With acetonitrile-0.1% phosphoric acid solution is mobile phase; The detection wavelength is 210nm.Number of theoretical plate calculates by the catalpol peak should be not less than 5000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the catalpol reference substance, adds mobile phase and make reference substance solution, promptly.
Chinese medicine composition phase content of the present invention is got in the preparation of need testing solution, gets about 1.0g, and accurate the title decides, and puts in the tool plug conical flask, the accurate methanol that adds claims to decide weight, and heating and refluxing extraction is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up, filter with methanol.Precision is measured subsequent filtrate 10ml, is concentrated near doing, and residue dissolves with mobile phase, is transferred in the measuring bottle, and is diluted to scale with mobile phase, shakes up, and filters, and gets subsequent filtrate, promptly.
Accurate respectively reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly.
The method of quality control of Chinese medicine composition of the present invention comprises one or more in following qualitative checking method and/or the quantitative detecting method:
(1) qualitative detection of Flos Farfarae
Get the pharmaceutical preparation of the present invention that is equivalent to crude drug 10.5g, porphyrize, the 25ml that adds diethyl ether makes dissolving, and supersound process 40 minutes is filtered, and filtrate is waved to 1.5ml, as need testing solution.Other Flos Farfarae control medicinal material 1g that withdraws the money shines medical material solution in pairs with legal system.According to thin layer chromatography test, draw each 25 μ l of above-mentioned two kinds of solution, respectively with same silica gel g thin-layer plate on, be developing solvent with 4: 1 ratio normal hexane-ethyl acetates, launch, take out, dry, spray is with vanillin concentrated sulphuric acid test solution, hot blast blow develop the color to speckle clear.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(2) qualitative detection of Semen Oroxyli
Get the pharmaceutical preparation of the present invention that is equivalent to crude drug 4g, porphyrize takes by weighing 1g, adds 50 milliliters of dehydrated alcohol ultrasonic 10 minutes, filters, and the filtrate evaporate to dryness adds 1 milliliter of dissolving of dehydrated alcohol as test sample.Other gets Semen Oroxyli control medicinal material 2g, adds 50 milliliters of dehydrated alcohol ultrasonic 10 minutes, filters, and the filtrate evaporate to dryness adds 1 milliliter of dehydrated alcohol and dissolves medical material solution in contrast.According to thin layer chromatography test, draw above-mentioned sample solution 15 μ l, control medicinal material solution 5 μ l are respectively and on the same silica gel g thin-layer plate, with 9: 1 ratio cyclohexane extraction-ethyl acetate was developing solvent, launched, and took out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(3) qualitative detection of Radix Ophiopogonis
Get the pharmaceutical preparation of the present invention that is equivalent to crude drug 10.5g, porphyrize adds 20 milliliters of the chloroform-methanols of 70: 30 ratios, soaked 3 hours, and ultrasonic 30 minutes, filter, evaporate to dryness is with 0.5 milliliter of dissolving of chloroform, as need testing solution.Other gets control medicinal material 2g Radix Ophiopogonis, shreds, with 20 milliliters of the chloroform-methanols of 70: 30 ratios, soaked 3 hours, and ultrasonic 30 minutes, filter, evaporate to dryness is with 0.5 milliliter of dissolving of chloroform, medical material solution in contrast.According to thin layer chromatography test, draw above-mentioned solution 10 μ l respectively, respectively with same silica gel g thin-layer plate on, be developing solvent with 5: 1 ratio normal hexane-ethyl acetate, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, hot blast blow develop the color to speckle clear.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(4) detection by quantitative of n-butyl alcohol extractum
Get the pharmaceutical preparation of the present invention that is equivalent to crude drug 8.5g, porphyrize is got powder 2g, the accurate title, decide, and the accurate methanol 50ml that adds claims to decide weight, put in the water-bath reflux 1 hour, and put coldly, supply the weight that subtracts mistake with methanol, filter, get subsequent filtrate 25ml, put in the evaporating dish that is dried to constant weight, evaporate to dryness, residue add water 25ml, make dissolving, with water saturated n-butanol extraction 3 times, each 25ml merges n-butyl alcohol liquid, put in the evaporating dish that is dried to constant weight, evaporate to dryness is 105 ℃ of dryings 3 hours, in the dislocation exsiccator, placed 30 minutes, weight decided in accurate rapidly title, calculates, promptly.
Chinese medicine composition of the present invention is pressed dry product and is calculated, and contains the n-butyl alcohol extractum and must not be less than 5.0%.
(5) detection by quantitative of harpagoside:
According to high effective liquid chromatography for measuring.
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With the acetonitrile is mobile phase A, is Mobile phase B with 1% acetum, and the regulation in the according to the form below is carried out gradient elution; The detection wavelength is 278nm.Number of theoretical plate calculates by the harpagoside peak should be not less than 5000.
| Time (minute) | Mobile phase A (%) | Mobile phase B (%) |
| 0～20 | 20→50 | 80→50 |
| 20～25 | 50→20 | 50→80 |
It is an amount of that the preparation precision of reference substance solution takes by weighing the harpagoside reference substance, adds 30% methanol and make the solution that every 1ml contains 10 μ g, promptly.
The preparation of need testing solution is got Chinese medicine composition of the present invention and is equivalent to crude drug 4.0g, and porphyrize is got about 1.0g, the accurate title, decide, and puts in the tool plug conical flask, the accurate 30% methanol 50ml that adds, close plug claims to decide weight, soaks after 1 hour, at power 500W, supersound process is 30 minutes under the frequency 40kHz, puts cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with 30% methanol, filter, get subsequent filtrate, promptly.
Inaccurate reference substance solution and each the 20 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Chinese medicine composition of the present invention is equivalent to crude drug 4.0g, contains harpagoside (C
24H
30O
11) must not be less than 0.18mg.
(6) detection by quantitative of catalpol
According to high effective liquid chromatography for measuring.
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With 1: 99 ratio acetonitrile-0.1% phosphoric acid solution was mobile phase; The detection wavelength is 210nm.Number of theoretical plate calculates by the catalpol peak should be not less than 5000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the catalpol reference substance, adds mobile phase and make the solution that every 1ml contains 10 μ g, promptly.
The preparation of need testing solution is got Chinese medicine composition of the present invention and is equivalent to crude drug 4.0g, and porphyrize is got about 1.0g, the accurate title, decide, put in the tool plug conical flask, the accurate methanol 25ml that adds claims to decide weight, heating and refluxing extraction 1.5 hours, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, filter.Precision is measured subsequent filtrate 10ml, is concentrated near doing, and residue dissolves with mobile phase, is transferred in the 10ml measuring bottle, and is diluted to scale with mobile phase, shakes up, and filters, and gets subsequent filtrate, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Chinese medicine composition of the present invention is equivalent to crude drug 4.0g, contains catalpol (C
15H
22O
10) must not be less than 0.25mg.
The specific embodiment
Following examples and test example are used to further specify but are not limited to the present invention
The test of test example 1 technical study
When determining the preparation technology of Chinese medicine composition of the present invention, according to the characteristics of the contained active ingredient of each flavour of a drug and the consideration of energy savings, determine that Radix Scrophulariae, the Radix Stemonae (system), Radix Asparagi, Cortex Moutan, Radix Ophiopogonis, Semen Oroxyli, Radix Rehmanniae, Radix Isatidis, Fructus Canarii, Periostracum Cicadae water extraction get final product, Flos Farfarae adopts full the pulverizing to be used as medicine.The kind of adjuvant and consumption are selected, the concrete quantification of art for coating, to the ageing of the quality stability that improves medicine of the present invention, safety, production and to the saving of the energy significance meaning are arranged all.
One, amount of water test
Press three parts of medical materials of recipe quantity configuration, every part contains Radix Scrophulariae 170g, the Radix Stemonae (system) 130g, Radix Asparagi 120g, Cortex Moutan 50g, Radix Ophiopogonis 70g, Semen Oroxyli 70g, Radix Rehmanniae 70g, Radix Isatidis 210g, Fructus Canarii 140g, Periostracum Cicadae 50g, and be divided into three groups and do experiment: first group of amount of water is respectively 10 times of amounts, 8 times of amounts; Second group of amount of water is 8 times of amounts, 6 times of amounts; The 3rd group of amount of water is 6 times of amounts, 4 times of amounts.With the paste volume is that index is determined amount of water.The results are shown in Table 1
Table 1: amount of water result of the test
| The group number | 1 | 2 | 3 |
| Paste volume (g) | 219.45 | 248.9 | 252.7 |
| Paste-forming rate (%) | 23.1 | 26.2 | 26.6 |
Above result shows: be that 8 times of amounts of index amount of water, 6 times of amount extractions are complete substantially with the paste volume, be defined as 8 times of amounts, 6 times of amounts according to the needs of production amount of water.
Two, the kind and the consumption that add adjuvant
Take by weighing according to above-mentioned selection process and extract raw medicinal material, after extracting solution concentrates, Flos Farfarae pulverizing medicinal materials to 100 order is added, mixing, drying is crushed to 80 orders, adds appropriate amount of auxiliary materials, granulate, drying, granulate adds 0.5% magnesium stearate again, tabletting, promptly.By comparing difficulty or ease, the tablet appearance of tabletting, select proper supplementary material and supplementary product consumption ratio, the results are shown in following table 2:
Table 2 adjuvant is selected result of the test
As can be seen from the above table, selecting to add adjuvant during the preparation tablet is sucrose, and addition is 1: 0.08, promptly can reach the requirement of preparation tablets.Promptly add adjuvant sucrose, its prescription consumption is 17g.
Three, art for coating
1 sealing coat: place coating pan to roll plain sheet, add to mix slurry (35% Resina persicae: 70% syrup=1: 5) make and evenly adhere to unilateral going up (plain sheet: mix slurry=50g: 1m1), the blowing hot-air drying, for preventing that tablet is inter-adhesive or sticking on the coating pan, add Pulvis Talci, 40～50 ℃ of hot blasts are dry down, twice of repetitive operation.
2 sub-coats: make slice, thin piece continue in coating pan, to roll, add 70% syrup, after making the even moistening of sheet sub-surface, add Pulvis Talci, make it to adhere to the sheet sub-surface, continue to roll and blowing dry (50～55 ℃) repetitive operation, till the slice, thin piece faceted pebble disappears, heavy by plain sheet: 70% syrup: Pulvis Talci=feed intake at 3: 1.7: 1.
3 sugarcoating layers: slice, thin piece is rolled in coating pan, add 70% syrup (plain sheet: 70% syrup=15: 1, the syrup addition is descending successively decreases), the sheet sub-surface is slowly dry, forms fine and smooth sugar crystal clothing layer, increases clothing layer fastness and sweet taste.
4 coloured sugarcoating layers: be diluted to the mill base of 2mg/ml with 70% syrup, mill base is diluted to variable concentrations with 70% syrup, concentration is ascending, adds coating pan, and is dry layer by layer.Plain sheet and pigment amount ratio are 7.5kg: 1g.
5 polishings: for making the coated tablet surface-brightening attractive in appearance, have moisture-proof role concurrently, add Cera Chinensis, add, rotate coating pan Cera Chinensis is wrapped on the slice, thin piece equably, take out coated tablet by plain sheet: Cera Chinensis=3kg: 5g, dry 24 hours, promptly.
The 2 method of quality control experimental studies of test example
Medicine of the present invention has the kinds of traditional Chinese medicines crude drug to process through extraction, grope by a large amount of tests, the thin layer chromatography discrimination method of determining Flos Farfarae, Semen Oroxyli, Radix Ophiopogonis is repeatability, good stability not only, and reliable results is noiseless, in the Radix Scrophulariae in harpagoside, the Radix Rehmanniae foundation of catalpol content assay method then further improved the controllability of drug quality of the present invention, an assay that in checking, has added the n-butyl alcohol extractum, just further perfect drug quality control method of the present invention.
1, the discriminating of Flos Farfarae
1) preparation of need testing solution:
Get according to 10 of the medicinal tablets of the present invention of embodiment 1 preparation for every part, remove sugar-coat, porphyrize adds ethanol, ether, chloroform respectively, and supersound process is filtered, and filtrate is waved to 1.5ml, as need testing solution.Be equipped with control medicinal material solution with legal system.
Negative sample according to the scarce Flos Farfarae of embodiment 1 preparation prepares negative control product solution according to the need testing solution preparation method again.
Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 25 μ l of above-mentioned three kinds of solution, respectively with same silica gel g thin-layer plate on, with normal hexane-ethyl acetate (4: 1) is developing solvent, launch, take out, dry, spray is with vanillin concentrated sulphuric acid test solution, and it is clear that hot blast blows to the speckle colour developing.Relatively more different the extraction solvent and extraction time, gained need testing solution and the color developing effect of control medicinal material solution on lamellae the results are shown in following table:
The preparation of table 3 need testing solution
As can be seen from the above table, during with ether supersound extraction 40min, test sample is all clear with each mottle colour developing of control medicinal material relevant position, good separating effect, and negative noiseless.Empirical tests, this method favorable reproducibility, Pass Test requirement.
2) selection of developing solvent
Prepare need testing solution, control medicinal material solution and negative control product solution according to above-mentioned method for optimizing, test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), drawing each 25 μ l of above-mentioned three kinds of solution, respectively and on the same silica gel g thin-layer plate, 2: 3,3: 2,3: 1,4: 1 was developing solvent with normal hexane-ethyl acetate, launch, take out, dry, spray is with vanillin concentrated sulphuric acid test solution, it is clear that hot blast blows to the speckle colour developing, relatively the expansion effect of each speckle on lamellae.The results are shown in following table:
The selection of table 4 developing solvent
| The developing solvent proportioning | 2∶3 | ?3∶2 | ?3∶1 | ?4∶1 |
| Launch effect | Each speckle separating effect is very poor, disturbs big. | Each speckle separating effect is very poor, disturbs big. | Each speckle separating effect is very poor, disturbs big. | Each speckle colour developing is clear, and good separating effect is noiseless. |
As can be seen from the above table, be at 4: 1 developing solvent with normal hexane-ethyl acetate, each speckle colour developing is clear, good separating effect, and negative noiseless, the Pass Test requirement.
2. the discriminating of Radix Ophiopogonis
We grope having carried out the thin layer discrimination method Radix Ophiopogonis in the medicine of the present invention with reference to medical material discrimination method under 2005 an editions Chinese Pharmacopoeias items Radix Ophiopogonis, but sample with Radix Ophiopogonis control medicinal material do not have corresponding speckle, and feminine gender has interference.We are conversion developing solvent on this basis again, and has carried out the check and negative investigation of three batch samples, has set up the discrimination method of Radix Ophiopogonis, and the result is as follows:
Table 5 differentiates that developing solvent selects test Radix Ophiopogonis
| The developing solvent proportioning | Toluene-methanol-glacial acetic acid (80: 5: 0.1) | Chloroform-ethyl acetate (5: 1) | Normal hexane-ethyl acetate (8: 1) | Normal hexane-ethyl acetate (5: 1) |
| Launch effect | Test sample with Radix Ophiopogonis control medicinal material do not have corresponding speckle, and negative | Test sample with Radix Ophiopogonis control medicinal material do not have corresponding speckle, and negative | Each speckle separating effect is very poor, the negative interference greatly. | Each speckle colour developing is clear, and good separating effect is noiseless. |
| Interference is arranged. | Disturb big. |
So determine that the thin layer discrimination method of Radix Ophiopogonis in the medicine of the present invention is as follows:
Get the pharmaceutical preparation of the present invention that is equivalent to raw medicinal material 10.5g, porphyrize, 20 milliliters of chloroform-methanols (70: 30) soaked 3 hours, and ultrasonic 30 minutes, filter, evaporate to dryness is with 0.5 milliliter of dissolving of chloroform, as need testing solution.Other gets control medicinal material 2g Radix Ophiopogonis, shreds, with 20 milliliters of chloroform-methanols (70: 30), soaked 3 hours, and ultrasonic 30 minutes, filter, evaporate to dryness is with 0.5 milliliter of dissolving of chloroform, medical material solution in contrast.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw above-mentioned solution 10 μ l respectively, respectively with same silica gel g thin-layer plate on, with normal hexane-ethyl acetate (5: 1) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
3. the discriminating of Semen Oroxyli
We have carried out the thin layer discrimination method with reference to medical material discrimination method under 2005 editions Chinese Pharmacopoeias Semen Oroxyli items to the Semen Oroxyli in the medicine of the present invention and have groped, but sample does not have corresponding speckle with the Semen Oroxyli control medicinal material, and feminine gender has interference.We are conversion developing solvent on this basis again, and has carried out the check and negative investigation of three batch samples, has set up the discrimination method of Radix Ophiopogonis, and the result is as follows:
Table 6 Semen Oroxyli is differentiated developing solvent selection test
| The developing solvent proportioning | N-butyl alcohol-acetic acid-water (6: 1.5: 2.5) | Chloroform-ethyl acetate (9: 1) | Cyclohexane extraction-ethyl acetate (6: 1) | Cyclohexane extraction-ethyl acetate (9: 1) |
| Launch effect | Test sample does not have corresponding speckle with the Semen Oroxyli control medicinal material, and feminine gender has interference. | Test sample with Radix Ophiopogonis control medicinal material do not have corresponding speckle, and negative disturb big. | Each speckle separating effect is very poor, the negative interference greatly. | Each speckle colour developing is clear, and good separating effect is noiseless. |
So determine that the thin layer discrimination method of Semen Oroxyli in the medicine of the present invention is as follows:
Get the pharmaceutical preparation of the present invention that is equivalent to raw medicinal material 4g, porphyrize takes by weighing 1g, adds 50 milliliters of dehydrated alcohol ultrasonic 10 minutes, filters, and the filtrate evaporate to dryness adds 1 milliliter of dissolving of dehydrated alcohol as test sample.Other gets Semen Oroxyli control medicinal material 2g, adds 50 milliliters of dehydrated alcohol ultrasonic 10 minutes, filters, and the filtrate evaporate to dryness adds 1 milliliter of dehydrated alcohol and dissolves medical material solution in contrast.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw above-mentioned sample solution 15 μ l, control medicinal material solution 5 μ l, respectively with same silica gel g thin-layer plate on, be developing solvent with cyclohexane extraction-ethyl acetate (9: 1), the expansion, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
4, the assay of n-butyl alcohol extractum
Get the pharmaceutical preparation of the present invention that is equivalent to raw medicinal material 8.5g, porphyrize is got powder 2g, the accurate title, decide, and the accurate methanol 50ml that adds claims to decide weight, put in the water-bath reflux 1 hour, and put coldly, supply the weight that subtracts mistake with methanol, filter, get subsequent filtrate 25ml, put in the evaporating dish that is dried to constant weight, evaporate to dryness, residue add water 25ml, make dissolving, with water saturated n-butanol extraction 3 times, each 25ml merges n-butyl alcohol liquid, put in the evaporating dish that is dried to constant weight, evaporate to dryness is 105 ℃ of dryings 3 hours, in the dislocation exsiccator, placed 30 minutes, weight decided in accurate rapidly title, calculates, promptly.
According to above assay method, 3 batches of medicines of the present invention according to embodiment 1 preparation to be carried out extract content measure, measurement result is as follows:
Table 7 extract content measurement result
| Lot number | Extract content (%) |
| 01 | 8.24％ |
| 02 | 8.43％ |
| 03 | 8.87％ |
According to above measurement result, this method good stability, simple and easy to do, so being pressed dry product, calculates medicine of the present invention, contain the n-butyl alcohol extractum and must not be less than 5.0%.
5, assay
(1) assay of harpagoside in the Radix Scrophulariae
1) chromatographic condition chromatographic column: Yi Lite C18 chromatographic column (4.6 * 200ram, 51xm); Mobile phase: the A acetonitrile, the B1% acetum carries out gradient elution by table 2.
Table 8 mobile phase ratio
| Time (min) | A(％) | B(％) |
| 0～20 | 20→50 | 80→50 |
| 20～25 | 50→20 | 50→80 |
Flow velocity: 1mL/min; Column temperature: 35 ℃; Detect wavelength: 278nm.Number of theoretical plate: should be not less than 5000 by the calculating of harpagoside peak.
2) it is an amount of that the harpagoside reference substance is got in the preparation of reference substance solution, adds 30% methanol and make the solution that every 1ml contains harpagoside 10 μ g, promptly.
3) it is an amount of that the medicine of the present invention for preparing according to embodiment 1 is got in the preparation of need testing solution, removes sugar-coat, and porphyrize is got 1.0g, the accurate title, decide, and puts in the tool plug conical flask, accurate 30% methanol 50ml, the close plug of adding, claim to decide weight, behind the immersion 1h, supersound process (power 5000W, frequency 40kHz) 30rain takes out, and puts cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with 30% methanol, filter, get subsequent filtrate, promptly.Respectively accurate draw reference substance solution and need testing solution each 201 ~ 1, inject high performance liquid chromatograph, measure, write down the chromatogram of 25min, promptly.
4) the negative blank sample that embodiment 1 preparation lacks Radix Scrophulariae is pressed in the preparation of negative control product solution, with test sample preparation method negative control solution.
5) accurate respectively each the 10 μ l of need testing solution, negative control solution and reference substance solution that draw of specificity test inject chromatograph of liquid, the record chromatogram.By chromatogram as seen, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on the chromatographic peak of identical retention time is arranged, negative test is noiseless.
6) the accurate absorption of the investigation of linear relationship concentration is harpagoside reference substance solution 5,10,15,20, the 25 μ l injection high performance liquid chromatograph of 10 μ g/ml, measure its peak area integrated value, with sample size is that horizontal seat peak area integrated value is a vertical coordinate, the drawing standard curve, its regression equation is: Y=1416.8x+12864, r=0.9998.The result shows that harpagoside has good linear relationship in 50-250 μ g scope.
Table 9 linear relationship is investigated
| Sample size (μ l) | 5 | 10 | 15 | 20 | 25 |
| Peak area | ?20124 | 26887 | 34032 | 41099 | 48437 |
7) the accurate same need testing solution (according to the test sample of embodiment 1 preparation) of drawing of precision test repeats sample introduction 5 times, measures its peak area, RSD=1.43%.The result shows that this method precision is good.
Table 10 precision is investigated
| Sample | 1 | 2 | 3 | 4 | 5 |
| Peak area | ?21754 | 21364 | 22178 | 22038 | 21881 |
| RSD | 1.43％ | ||||
8) accurate same need testing solution (according to the test sample of embodiment 1 preparation) the 20 μ l that draw of stability test respectively at 0,4,8,12, the 16h sample introduction, measure its peak area integrated value, and the peak area meansigma methods is 21846.6.RSD=1.57%, result show that need testing solution peak area integrated value in 16h is basicly stable.
Table 11 study on the stability
| Sample | 1 | 2 | 3 | 4 | 5 |
| Peak area | ?21566 | 22314 | 21498 | 22063 | 21792 |
| RSD | ?1.57％ | ||||
9) replica test is got 5 parts in same lot number sample (according to the test sample of embodiment 1 preparation), measures 5 times in accordance with the law, and average content is 0.2646mg/g, RSD; 1.61%, the result shows that this method repeatability better.
Table 12 repeatability is investigated
| Sample | 1 | 2 | 3 | 4 | 5 |
| Content mg/g | 0.2674 | 0.2598 | 0.2614 | 0.2702 | 0.2643 |
| RSD | 1.61％ | ||||
10) to take by weighing known content be the about 1.0g of 0.2637mg/g sample (according to the test sample of embodiment 1 preparation) to the recovery test precision, and totally 5 parts, accurate respectively adding harpagoside reference substance solution (1.5mg/ml) 1ml measures content in accordance with the law, the results are shown in Table 13.
Table 13 average recovery measurement result
| Numbering | Sampling amount (g) | Harpagoside amount (mg) in the sample | Add harpagoside amount (mg) | Actual measurement harpagoside amount (mg) | The response rate (%) | RSD |
| 1 | 1.0321 | 0.2722 | 1.5 | 1.7302 | 97.63 | 1.55％ |
| 2 | 1.0549 | 0.2782 | 1.5 | 1.8027 | 101.38 | |
| 3 | 1.0681 | 0.2817 | 1.5 | 1.7410 | 97.72 | |
| 4 | 1.0938 | 0.2884 | 1.5 | 1.7807 | 99.57 | |
| 5 | 1.0122 | 0.2669 | 1.5 | 1.7489 | 98.98 |
The result shows that this method average recovery is better.
From above methodological study result as can be seen, all Pass Test requirements such as the content assaying method precision of harpagoside, repeatability, stability in the Radix Scrophulariae are so determine that the content to measure harpagoside in the Radix Scrophulariae is one of method of quality control.
(2) assay of catalpol in the Radix Rehmanniae
1 instrument and test solution
Instrument: Aglient 1100 HPLC analyzers, chem station for LC chromatographic data process software.Reagent: methanol, second is fine is chromatographically pure, and water is water for injection, and other reagent are analytical pure.Reference substance: catalpol reference substance (for assay usefulness, Nat'l Pharmaceutical ﹠ Biological Products Control Institute provides).Sample: according to the medicine of the present invention of embodiment 1 preparation.
2 chromatographic conditions
Chromatographic column be the C18 chromatographic column (Type Waters, 4.6 * 250mm), mobile phase is that second is fine: methanol: water (6: 3: 150), the detection wavelength is 210nm, flow velocity is 0.8mldmin.
3 detect wavelength determination
Get the catalpol reference substance, measure its absorption curve at 200 ~ 400nm with spectrophotometer.Find that it has absorption maximum at the 210nm place, so select 210nm for detecting wavelength.
4 experimental techniques
4.1 the preparation precision of reference substance solution takes by weighing catalpol reference substance 4.58mg, puts in the 100mL volumetric flask, adds dissolve with methanol and is diluted to scale, shakes up, and promptly gets (every 1mL reference substance solution contains catalpol 0.0458mg).
4.2 it is an amount of that the preparation of need testing solution takes by weighing according to the medicine of the present invention of embodiment 1 preparation, removes sugar-coat, porphyrize, get 2g, accurate claim surely, put that to add methanol in the apparatus,Soxhlet's an amount of, extract 4h, take out, put cold, filter, methanol extract liquid low temperature reclaims methanol to about 10mL, and methanol extract liquid quantitatively is transferred in the 25mL volumetric flask, adds methanol and is diluted to scale, shake up, as need testing solution.
4.3 the negative blank sample that embodiment 1 preparation lacks Radix Rehmanniae is pressed in the preparation of negative control solution, with test sample preparation method negative control solution.
4.4 the accurate respectively reference substance solution of drawing of assay method, need testing solution, each 20uL of negative control product solution injects chromatograph of liquid, measures, promptly.Disturbing does not appear in the relevant position of test sample catalpol in negative sample solution.
4.5 the investigation precision of linear relationship takes by weighing catalpol reference substance solution (0.235mg/mL) 1,5,9,13,17,20mL, put in the 20mL volumetric flask, add methanol to scale, concentration be 0.01175,0.05875,0,1058,0.1528,0.1998, the catalpol reference substance solution of 0.235mg/mL, draw above-mentioned 6 kinds of each 20uL of solution respectively, inject hplc determination, regression equation is A=94153C+198.11, correlation coefficient, r=0,9996.
Table 14 linear relationship is investigated
| Concentration (mg/ mL) | 0.01175 | 0.05875 | 0.1058 | 0.1528 | 0.1998 | 0.235 |
| Peak area | 1304.4 | 5729.6 | 10159.5 | 14584.7 | 19009.9 | 22324.1 |
The result shows that catalpol is good in the scope internal linear relation of 0.235-4.70 μ g.
4.6 replica test is got same batch sample (according to the medicine of the present invention of embodiment 1 preparation), parallel preparation 6 duplicate samples press sample determination method mensuration, 0.306mg/g as a result, and RSD is 1.59%.
Table 15 repeatability is investigated
| Sample | 1 | 2 | 3 | 4 | 5 | 6 |
| Content mg/g | 0.310 | 0.304 | 0.311 | 0.309 | 0.302 | 0.299 |
| RSD | 1.59％ | |||||
4.7 accurate same catalpol reference substance solution (0.0458mg/mL) 20uL that draws of precision test injects chromatograph of liquid, METHOD FOR CONTINUOUS DETERMINATION 6 times is measured peak area value, and RSD is 0.80%.
Table 16 precision is investigated
| Sample | 1 | 2 | 3 | 4 | 5 | 6 |
| Peak area | ?29568 | 29267 | 29134 | 29075 | 29664 | 29359 |
| RSD | ?0.80％ | |||||
4.8 the average recovery test is by the requirement of average recovery test, with same batch sample (according to the medicine of the present invention of embodiment 1 preparation) preparation need testing solution, precision is measured 4 parts of 5mL need testing solutions, put respectively in the 10mL measuring bottle, add catalpol reference substance solution (0.0458mg/mL) respectively and put scale, press the sample determination method, get the test sample 5mL that does not add reference substance and put in the volumetric flask with method and measure, the total content of getting 5mL is 1.40% for background values RSD.See table 17 for details.
Table 17 response rate experimental result
| Sample size/(mg/g) | Addition/mg | Measured value/mg | The response rate (%) | Average recovery rate (%) |
| 0.2935 | 0.2290 | 0.5118 | 95.33 | 97.27 |
| 0.5183 | 98.17 | |||
| 0.5164 | 97.34 | |||
| 0.5185 | 98.25 |
From above methodological study result as can be seen, all Pass Test requirements such as the content assaying method precision of catalpol, repeatability, stability in the Radix Rehmanniae are so determine that the content to measure catalpol in the Radix Rehmanniae is one of method of quality control.
The test of test example 3 pharmacodynamic studies
1 experiment material
1.1 medicine is according to pharmaceutical preparation I of the present invention, the II of embodiment 1,2 preparations; Yanyan slice (specification: 0.25g/ sheet (coated tablet), GANKANG pharmaceutical Co. Ltd in Jilin produces; Aspirin is by Shenyang Medical College production; Ammonium chloride is analytical pure; According to train of thought orchid, 5-hydroxy tryptamine Fluka import packing, Shanghai chemical reagent purchasing and supply station packing factory.
1.2 animal Wistar rat, ICR mice and SD rat, ♀ ♂ all uses.
2 methods and result
Get 60 of rats, body weight 200～250g, male and female half and half, 10 every group 2.1 suppress the effect of capillary permeability.Be divided into 6 groups at random, drug component of the present invention Gei medicine I heavy dose of the present invention not organized 70g/kg, small dose group 35g/kg, medicine II small dose group 35g/kg of the present invention (the contained crude drug amount of medicinal liquid), the saline control group is given normal saline 20ml/kg, the aspirin group is given aspirin 268mg/kg, the positive drug matched group is given Yanyan slice 37g/kg (the contained crude drug amount of medicinal liquid), each is organized behind ig administration or saline 30min, at the 5-hydroxy tryptamine 0.1ml of rat back center line left side subcutaneous injection 1 μ g/ml, iv1% is according to the blue 4ml/kg of the train of thought immediately.Put to death animal behind the 15min, the painted skin in back is cut and shredded put into 3ml normal saline-acetone (3: 7) mixed liquor, place 24h, get supernatant, with 721 spectrophotometers (610nm) photometry density.The results are shown in Table 18.
Table 18 suppresses the effect of capillary permeability
| Group | Dosage | Optical density value (x ± s) |
| The saline control group | 20ml/kg | 0.1233±0.0526 |
| The aspirin group | 268mg/kg | 0.0611±0.0224** |
| The positive drug matched group | 37g/kg | 0.0747±0.0224* |
| Medicine group I heavy dose of the present invention | 70g/kg | 0.0570±0.0218** |
| Medicine group I low dose of the present invention | 35g/kg | 0.0628±0.0208** |
| Medicine group II low dose of the present invention | 35g/kg | 0.0651±0.0236* |
Annotate: n=10, compare * * P＜0.01, * P＜0.05 with the saline control group
Each group of medicine of the present invention all has inhibitory action to capillary permeability due to the 5-hydroxy tryptamine, the excellent positive control medicine of the inhibitory action of medicine of the present invention, and the effect of medicine I of the present invention is better than medicine II of the present invention.
2.2 influence 60 of extracting male Wistar rats to what carrageenin caused rat paw edema, body weight 140～160g, grouping and administration are the same, 1h after the administration, in the subcutaneous injection 1% carrageenin 0.1ml/ of the right sufficient sole of the foot of rat only.Cause scorching back 1～6h and measure sufficient sole of the foot volume respectively, calculate swelling value (causing the sufficient sole of the foot difference in volume in scorching front and back).The results are shown in Table 19.
Table 19 pair carrageenin causes the influence of rat paw edema
| Group | Dosage | The swelling value (ml, x ± s) | |||||
| 1h | 2h | 3h | 4h | 5h | 6h | ||
| The saline control group | 20ml/kg | 0.36± 0.12 | 0.66± 0.13 | 0.55± 0.19 | 0.51± 0.09 | 0.63± 0.08 | 0.36± 0.08 |
| The aspirin group | 268mg/kg | 0.21± 0.12** | 0.33± 0.12** | 0.26± 0.13** | 0.22± 0.13** | 0.20± 0.12** | 0.18± 0.11* |
| The positive drug matched group | 37g/kg | 0.26± 0.12 | 0.42± 0.12* | 0.35± 0.11* | 0.32± 0.13 | 0.25± 0.11* | 0.20± 0.10 |
| Medicine group I heavy dose of the present invention | 70g/kg | 0.22± 0.09** | 0.34± 0.10** | 0.27± 0.08** | 0.21± 0.07** | 0.14± 0.09** | 0.10± 0.10* |
| Medicine group I low dose of the present invention | 35g/kg | 0.24± 0.10* | 0.36± 0.10** | 0.31± 0.09** | 0.23± 0.11** | 0.18± 0.12** | 0.18± 0.11* |
| Medicine group II low dose of the present invention | 35g/kg | 0.27± 0.12 | 0.39± 0.13* | 0.32± 0.12* | 0.25± 0.12* | 0.21± 0.11* | 0.18± 0.10* |
Annotate: n=10, compare * * P＜0.01, * P＜0.05 with the saline control group
Each group of medicine of the present invention causes rat paw edema to carrageenin all inhibitory action, and the inhibitory action of medicine of the present invention is better than the positive control medicine, and the effect of medicine I of the present invention is better than medicine II of the present invention.
2.3 to outgrowth 60 of the extracting male Wistar rats that influence of rat granuloma, body weight 140-160g, grouping and administration are the same.At the descending back of narcotism median incision 1cm, at the subcutaneous diameter 9mm that buries of left shoulder, thick 1.5mm, the aseptic filter paper sheet of heavy 9.25mg.Administration every day 2 times, continuous 7 days, took out granulation tissue on the 8th day, weigh behind 60 ℃ of dry 24h, obtain average and the suppression ratio of respectively organizing net weight.The results are shown in Table 20.
The table 20 pair outgrowth influence of rat granuloma
| Group | Dosage | The granulation tissue net weight (mg, x ± s) | Suppression ratio (%) |
| The saline control group | 20ml/kg | 76.9±10.6 | -- |
| The aspirin group | 268mg/kg | 41.9±9.0** | 45.5 |
| The positive drug matched group | 37g/kg | 49.2±11.2* | 36.0 |
| Medicine group I heavy dose of the present invention | 70g/kg | 41.0±8.2** | 46.7 |
| Medicine group I low dose of the present invention | 35g/kg | 44.1±11.0** | 42.6 |
| Medicine group II low dose of the present invention | 35g/kg | 46.9±8.0** | 39.7 |
Annotate: n=10, compare * * P＜0.01, * P＜0.05 with the saline control group
As can be seen from the above table, each group of medicine of the present invention all has inhibitory action to rat granuloma hypertrophy, and the inhibitory action of medicine of the present invention is significantly higher than the positive control medicine, and the effect of medicine I of the present invention is better than medicine II of the present invention.
2.4 to influence (capillary glass-tube method) the SD rat of rat expectoration amount, ♀ ♂ half and half, body weight 200～250g is divided into 6 groups at random, and 10 every group, the positive drug matched group is administration 37g/kg Yanyan slice and 1gkg ammonium chloride.Insert the normal sputum secretory volume in the 2h before the administration of capillary glass tube record, each group gives relative medicine with the 1mL/100g duodenum respectively then, continues the sputum secretory volume in the 2h after the record administration.Draw the effect of reducing phlegm that sputum length is estimated medicine with capillary tube.The results are shown in Table 21.
The influence of table 21 pair rat expectoration amount
| Group | Dosage (g*kg) | Expectoration amount (cm) | |
| In the preceding 2h of administration | After the administration in the 2h | ||
| The saline control group | L0mL/kg | 1.83±0.25 | 1.93±0.18 |
| Ammonium chloride | 1.0 | 1.86±0.23 | 3.03±0.31** |
| The positive drug matched group | 37g/kg | 1.84±0.29 | 2.11±0.20* |
| Medicine group I heavy dose of the present invention | 70g/kg | 1.81±0.16 | 3.15±0.30** |
| Medicine group I low dose of the present invention | 35g/kg | 1.88±0.39 | 2.94±0.29** |
| Medicine group II low dose of the present invention | 35g/kg | 1.89±0.30 | 2.82±0.40** |
The result shows that pharmaceutical composition of the present invention, ammonium chloride and the Yanyan slice of 3 kinds of dosage all can significantly increase the expectoration amount of rat, and the effect of medicine I of the present invention is better than medicine II of the present invention.
2.5 to strong aqua ammonia draw cough influence the ICR mice, ♀ ♂ half and half, body weight 20～24g is divided into 5 groups at random, 10 every group, the positive drug matched group is the 37g/kg Yanyan slice.Animal is all with 0.1mL/10g body weight ig administration, one day twice, continuous 5 times.The reference literature method is observed cough latent period (spraying finished to the time that begins to occur coughing) and the interior cough number of times of 3min behind 27% the strong aqua ammonia that mice feeds atomizing behind last administration 45min.The results are shown in Table 22.
Table 22 pair strong aqua ammonia draws the influence of coughing
| Group | Dosage (g*kg) | Cough latent period (s) | Cough number of times in the 30min |
| The saline control group | Equal-volume | 45.8±8.7 | ?75.3±6.5 |
| The positive drug matched group | 37g/kg | 48.1±10.3 | ?70.0±7.4 |
| Medicine group I heavy dose of the present invention | 70g/kg | 77.8±9.8* | ?46.1±5.9* |
| Medicine group I low dose of the present invention | 35g/kg | 57.7±15.0* | ?59.7±6.2 |
| Medicine group II low dose of the present invention | 35g/kg | 53.1±7.5 | ?62.3±5.1 |
This experimental result shows, medicine I high dose of the present invention can the significant prolongation cough latent period also reduce the cough number of times, in only prolong cough latent period during dosage, to the obviously influence of cough number of times unit, the cough latent period of medicine II of the present invention and cough time number average unit significant change.But it is better that medicine of the present invention and positive control medicine relatively draw the inhibitory action of coughing to strong aqua ammonia.
4 clinical trials of test example
Clinical data 150 routine chronic pharyngitiss all are the hospital outpatient patient, are divided into two groups at random, and 90 examples are organized in treatment, male 60 examples, women 30 examples; The oldest person 75 years old, minimum 12 years old; The course of disease 1 month～1 year.Matched group 60 examples, male 45 examples, women 15 examples, maximum 72 years old age, minimum 13 years old; The course of disease 1 month～1 year.Diagnostic criteria meets " traditional Chinese medical science common disease conventional treatment ".
Therapeutic Method treatment group is used the pharmaceutical preparation of the present invention according to embodiment 1 preparation, and is oral, 1 time 5,3 times on the 1st.Taking 10d continuously is 1 course of treatment, 1～3 the course of treatment observed result.The Yanyan slice that matched group adopts Jilin GANKANG pharmaceutical Co. Ltd to produce, the 0.25g/ sheet, 1d3 time, 1 time 5, taking 10d continuously is 1 course of treatment, 1～3 the course of treatment observed result.
Criterion of therapeutical effect is drafted with reference to chronic throat obstruction, chronic pharyngitis standard in " traditional Chinese medical science common disease conventional treatment ".Cure: subjective symptoms disappears, and pharyngeal congestion, edema disappear; Produce effects: symptom obviously alleviates, pharyngeal congestion, edema basic controlling; Effectively: symptom makes moderate progress, and pharyngeal congestion, edema obviously alleviate; Invalid: doing well,improving is slight or do not have improvement, and pharyngeal congestion water, swollen nothing obviously alleviate.
90 examples are organized in the therapeutic outcome treatment, clinical cure 23 examples, and produce effects 30 examples, effective 31 examples, invalid 6 examples, total effective rate is 93.33%.Matched group 60 examples, clinical cure 6 examples, produce effects 16 examples, effective 25 examples, invalid 13 examples, total effective rate is 78.33%.Two groups relatively have significant difference (P＜0.01).
Clinical research shows that Drug therapy chronic pharyngitis effect of the present invention is remarkable.
Specific embodiment
Embodiment 1
Radix Scrophulariae 170g Radix Asteris 130g Radix Asparagi 120g
Radix Arnebiae (Radix Lithospermi) 50g 70g Radix Ophiopogonis Flos Farfarae (system) 60g
Semen Oroxyli 70g Radix Rehmanniae 70g Flos Lonicerae 210g
Rhizoma Belamcandae 140g Fructus Arctii 50g Oleum menthae 0.5g
More than 12 the flavor, except that Oleum menthae, Flos Farfarae is crushed to 100 orders, sieves; Ten flavors such as all the other Radix Scrophulariaes decoct with water secondary, add 8 times of water gagings for the first time and decoct 3 hours, add 6 times of water gagings for the second time and decoct 2 hours, collecting decoction left standstill 24 hours, got supernatant, being condensed into relative density is the thick paste of 1.35 (60-70 ℃), mixes with Common Coltsfoot Flower, at drying under reduced pressure below 60 ℃, be crushed to 80 orders, add the sucrose of 25g, make granule, spray adds the 1.75g magnesium stearate, mixing with Oleum menthae, be pressed into 1000, sugar coating, promptly.
Embodiment 2
The Radix Scrophulariae 170g Radix Stemonae (system) 130g Radix Asparagi 120g
Cortex Moutan 50g 70g Radix Ophiopogonis Flos Farfarae (system) 60g
Semen Oroxyli 70g Radix Rehmanniae 70g Radix Isatidis 210g
Fructus Canarii 140g Periostracum Cicadae 50g Oleum menthae 0.5g
More than 12 the flavor, except that Oleum menthae, Flos Farfarae is crushed to 100 orders, sieves; Ten flavors such as all the other Radix Scrophulariaes decoct with water secondary, add 8 times of water gagings for the first time and decoct 3 hours, add 6 times of water gagings for the second time and decoct 2 hours, collecting decoction left standstill 24 hours, got supernatant, being condensed into relative density is the thick paste of 1.35 (60-70 ℃), mixes with Common Coltsfoot Flower, at drying under reduced pressure below 60 ℃, be crushed to 80 orders, add the sucrose of 25g, make granule, spray adds the 1.5g magnesium stearate, mixing with Oleum menthae, be pressed into 1000, sugar coating, promptly.
Embodiment 3
Radix Scrophulariae 150g Radix Asteris 120g Radix Asparagi 130g
Radix Arnebiae (Radix Lithospermi) 40g 80g Radix Ophiopogonis Flos Farfarae (system) 40g
Semen Oroxyli 80g Radix Rehmanniae 50g Flos Lonicerae 230g
Rhizoma Belamcandae 120g Fructus Arctii 40g Oleum menthae 0.4g
More than 12 the flavor, except that Oleum menthae, Flos Farfarae is crushed to 100 orders, sieves; Ten flavors such as all the other Radix Scrophulariaes decoct with water secondary, add 8 times of water gagings for the first time and decoct 3 hours, add 6 times of water gagings for the second time and decoct 2 hours, collecting decoction left standstill 24 hours, got supernatant, being condensed into relative density is the thick paste of 1.35 (60-70 ℃), mixes with Common Coltsfoot Flower, at drying under reduced pressure below 60 ℃, be crushed to 80 orders, add the sucrose of 15g, make granule, spray adds the 0.8g magnesium stearate, mixing with Oleum menthae, be pressed into 1000, sugar coating, promptly.
Embodiment 4
Radix Scrophulariae 180g Radix Asteris 150g Radix Asparagi 100g
Radix Arnebiae (Radix Lithospermi) 70g 50g Radix Ophiopogonis Flos Farfarae (system) 70g
Semen Oroxyli 50g Radix Rehmanniae 80g Flos Lonicerae 200g
Rhizoma Belamcandae 150g Fructus Arctii 70g Oleum menthae 0.6g
More than 12 the flavor, except that Oleum menthae, Flos Farfarae is crushed to 100 orders, sieves; Ten flavors such as all the other Radix Scrophulariaes decoct with water secondary, add 8 times of water gagings for the first time and decoct 3 hours, add 6 times of water gagings for the second time and decoct 2 hours, collecting decoction left standstill 24 hours, got supernatant, being condensed into relative density is the thick paste of 1.35 (60-70 ℃), mixes with Common Coltsfoot Flower, at drying under reduced pressure below 60 ℃, be crushed to 80 orders, add the sucrose of 15g, make granule, spray adds particle weight 0.8g magnesium stearate, mixing with Oleum menthae, be pressed into 1000, sugar coating, promptly.
Embodiment 5 is according to the method for quality control of the pharmaceutical preparation of the present invention of embodiment 1～4 preparation
Differentiate:
(1) get 10 of this product, remove sugar-coat, porphyrize, the 25ml that adds diethyl ether makes dissolving, and filter at ultrasonic place 40 minutes, and filtrate is waved to 1.5ml, as need testing solution.Other Flos Farfarae control medicinal material 1g that withdraws the money shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 25 μ l of above-mentioned two kinds of solution, respectively with same silica gel g thin-layer plate on, with normal hexane-ethyl acetate (4: 1) is developing solvent, launch, take out, dry, spray is with vanillin concentrated sulphuric acid test solution, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(2) get this product, remove sugar-coat, porphyrize takes by weighing 1g, adds 50 milliliters of dehydrated alcohol ultrasonic 10 minutes, filters, and the filtrate evaporate to dryness adds 1 milliliter of dissolving of dehydrated alcohol as test sample.Other gets Semen Oroxyli control medicinal material 2g, adds 50 milliliters of dehydrated alcohol ultrasonic 10 minutes, filters, and the filtrate evaporate to dryness adds 1 milliliter of dehydrated alcohol and dissolves medical material solution in contrast.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw above-mentioned sample solution 15 μ l, control medicinal material solution 5 μ l, respectively with same silica gel g thin-layer plate on, be developing solvent with cyclohexane extraction-ethyl acetate (9: 1), the expansion, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(3) sample thief is 10, removes sugar-coat, porphyrize, and 20 milliliters of chloroform-methanols (70: 30) soaked 3 hours, and ultrasonic 30 minutes, filter, evaporate to dryness is with 0.5 milliliter of dissolving of chloroform, as need testing solution.Other gets control medicinal material 2g Radix Ophiopogonis, shreds, with 20 milliliters of chloroform-methanols (70: 30), soaked 3 hours, and ultrasonic 30 minutes, filter, evaporate to dryness is with 0.5 milliliter of dissolving of chloroform, medical material solution in contrast.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw above-mentioned solution 10 μ l respectively, respectively with same silica gel g thin-layer plate on, with normal hexane-ethyl acetate (5: 1) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Check:
The n-butyl alcohol extractum takes by weighing this product, removes sugar-coat, porphyrize, get powder 2g, the accurate title, decide, the accurate methanol 50ml that adds, claim to decide weight, put in the water-bath reflux 1 hour, put cold, supply the weight that subtracts mistake with methanol, filter, get subsequent filtrate 25ml, put in the evaporating dish that is dried to constant weight, evaporate to dryness, residue add water 25ml, make dissolving, with water saturated n-butanol extraction 3 times, each 25ml, merge n-butyl alcohol liquid, put in the evaporating dish that is dried to constant weight evaporate to dryness, 105 ℃ of dryings 3 hours, in the dislocation exsiccator, placed 30 minutes, weight decided in accurate rapidly title, calculate, promptly.
This product is pressed dry product and is calculated, and contains the n-butyl alcohol extractum and must not be less than 5.0%.
Assay:
Radix Scrophulariae:
Measure according to high performance liquid chromatography (appendix VI D).
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With the acetonitrile is mobile phase A, is Mobile phase B with 1% acetum, and the regulation in the according to the form below is carried out gradient elution; The detection wavelength is 278nm.Number of theoretical plate calculates by the harpagoside peak should be not less than 5000.
| Time (minute) | Mobile phase A (%) | Mobile phase B (%) |
| 0～20 | 20→50 | 80→50 |
| 20～25 | 50→20 | 50→80 |
It is an amount of that the preparation precision of reference substance solution takes by weighing the harpagoside reference substance, adds 30% methanol and make the solution that every 1ml contains 10 μ g, promptly.
The preparation of need testing solution is got Chinese medicine composition of the present invention and is equivalent to crude drug 4.0g, and porphyrize is got about 1.0g, the accurate title, decide, and puts in the tool plug conical flask, the accurate 30% methanol 50ml that adds, close plug claims to decide weight, soaks after 1 hour, supersound process (power 500W, frequency 40kHz) 30 minutes is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with 30% methanol, filter, get subsequent filtrate, promptly.
Inaccurate reference substance solution and each the 20 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Chinese medicine composition of the present invention is equivalent to crude drug 4.0g, contains harpagoside (C
24H
30O
11) must not be less than 0.18mg.Radix Rehmanniae:
Measure according to high performance liquid chromatography (appendix VI D).
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With acetonitrile-0.1% phosphoric acid solution (1: 99) is mobile phase; The detection wavelength is 210nm.Number of theoretical plate calculates by the catalpol peak should be not less than 5000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the catalpol reference substance, adds mobile phase and make the solution that every 1ml contains 10 μ g, promptly.
The preparation of need testing solution is got Chinese medicine composition of the present invention and is equivalent to crude drug 4.0g, and porphyrize is got about 1.0g, the accurate title, decide, put in the tool plug conical flask, the accurate methanol 25ml that adds claims to decide weight, heating and refluxing extraction 1.5 hours, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, filter.Precision is measured subsequent filtrate 10ml, is concentrated near doing, and residue dissolves with mobile phase, is transferred in the 10ml measuring bottle, and is diluted to scale with mobile phase, shakes up, and filters, and gets subsequent filtrate, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Chinese medicine composition of the present invention is equivalent to crude drug 4.0g, contains catalpol (C
15H
22O
10) must not be less than 0.25mg..
Embodiment 7 capsules
Radix Scrophulariae 170g Radix Asteris 130g Radix Asparagi 120g
Radix Arnebiae (Radix Lithospermi) 50g 70g Radix Ophiopogonis Flos Farfarae (system) 60g
Semen Oroxyli 70g Radix Rehmanniae 70g Flos Lonicerae 210g
Rhizoma Belamcandae 140g Fructus Arctii 50g Oleum menthae 0.5g
More than 12 the flavor, except that Oleum menthae, Flos Farfarae is crushed to 100 orders, sieves; Ten flavors such as all the other Radix Scrophulariaes decoct with water three times, add 8 times of water gagings for the first time and decoct 3 hours, add 6 times of water gagings for the second time and decoct 2 hours, add 6 times of water gagings for the third time and decocted 2 hours, collecting decoction left standstill 30 hours, get supernatant, being condensed into relative density is the thick paste of 1.35 (60-70 ℃), mixes with Common Coltsfoot Flower, at drying under reduced pressure below 60 ℃, be crushed to 80 orders, add the sucrose of 25g, make granule, spray adds the 1.5g magnesium stearate with Oleum menthae, mixing, 1000 capsules of packing into, promptly.
Embodiment 8 granules
Radix Scrophulariae 170g Radix Asteris 130g Radix Asparagi 120g
Radix Arnebiae (Radix Lithospermi) 50g 70g Radix Ophiopogonis Flos Farfarae (system) 60g
Semen Oroxyli 70g Radix Rehmanniae 70g Flos Lonicerae 210g
Rhizoma Belamcandae 140g Fructus Arctii 50g Oleum menthae 0.5g
More than 12 the flavor, except that Oleum menthae, Flos Farfarae is crushed to 100 orders, sieves; Ten flavors such as all the other Radix Scrophulariaes decoct with water secondary, add 8 times of water gagings for the first time and decoct 3 hours, add 6 times of water gagings for the second time and decoct 2 hours, collecting decoction left standstill 24 hours, got supernatant, being condensed into relative density is the thick paste of 1.35 (60-70 ℃), mix with Common Coltsfoot Flower, add 250g starch, 500g sucrose again, mixing, make granule, spray is made the 1000g granule, promptly with Oleum menthae.
Embodiment 9 drop pills
Radix Scrophulariae 170g Radix Asteris 130g Radix Asparagi 120g
Radix Arnebiae (Radix Lithospermi) 50g 70g Radix Ophiopogonis Flos Farfarae (system) 60g
Semen Oroxyli 70g Radix Rehmanniae 70g Flos Lonicerae 210g
Rhizoma Belamcandae 140g Fructus Arctii 50g Oleum menthae 0.5g
More than 12 the flavor, except that Oleum menthae, Flos Farfarae is crushed to 100 orders, sieves; Ten flavors such as all the other Radix Scrophulariaes decoct with water secondary, add 8 times of water gagings for the first time and decoct 3 hours, add 6 times of water gagings for the second time and decoct 2 hours, collecting decoction left standstill 24 hours, got supernatant, being condensed into relative density is the thick paste of 1.35 (60-70 ℃), mix with Common Coltsfoot Flower, drying is crushed to 120 orders, even with fused Macrogol 4000 according to 1: 3 mixed, add the Oleum menthae mixing rapidly, drip and make drop pill, promptly.
Embodiment 10 syrups
Radix Scrophulariae 170g Radix Asteris 130g Radix Asparagi 120g
Radix Arnebiae (Radix Lithospermi) 50g 70g Radix Ophiopogonis Flos Farfarae (system) 60g
Semen Oroxyli 70g Radix Rehmanniae 70g Flos Lonicerae 210g
Rhizoma Belamcandae 140g Fructus Arctii 50g Oleum menthae 0.5g
More than 12 flavors, except that Oleum menthae, all the other Radix Scrophulariaes etc. ten decoct with water secondary simply, add for the first time 8 times of water gagings and decoct 3 hours, add for the second time 6 times of water gagings and decocted 2 hours, collecting decoction left standstill 24 hours, get supernatant, be concentrated in right amount, other gets sucrose 650g and adds water boil, after the dissolving, filter, concentrate and make syrup, with above-mentioned concentrated solution mixing, boil, put cold, add Oleum menthae, antiseptic and essence, and be diluted to 1000ml, promptly with cold boiled water.
Embodiment 11 buccal tablets
Radix Scrophulariae 170g Radix Asteris 130g Radix Asparagi 120g
Radix Arnebiae (Radix Lithospermi) 50g 70g Radix Ophiopogonis Flos Farfarae (system) 60g
Semen Oroxyli 70g Radix Rehmanniae 70g Flos Lonicerae 210g
Rhizoma Belamcandae 140g Fructus Arctii 50g Oleum menthae 0.5g
More than 12 the flavor, except that Oleum menthae, all the other Radix Scrophulariaes etc. ten decoct with water secondary simply, add for the first time 8 times of water gagings and decocted 3 hours, add 6 times of water gagings for the second time and decocted collecting decoction 2 hours, left standstill 24 hours, and got supernatant, concentrated relative density is the thick paste of 1.35 (60-70 ℃), add sucrose 750g, vanillin 1.5g, cyclamate 10g, citric acid 15g mixing, make granule, drying, granulate sprays into volatile oil, mixing, be pressed into 1000, promptly.
Embodiment 12
The Radix Scrophulariae 170g Radix Stemonae (system) 130g Radix Asparagi 120g
Cortex Moutan 50g 70g Radix Ophiopogonis Flos Farfarae (system) 60g
Semen Oroxyli 70g Radix Rehmanniae 70g Radix Isatidis 210g
Fructus Canarii 140g Periostracum Cicadae 50g Oleum menthae 0.5g
More than 12 the flavor, except that Oleum menthae, Flos Farfarae is crushed to 100 orders, sieves; Ten flavors such as all the other Radix Scrophulariaes add 8 times of water gagings and decocted 4 hours, filter, and decocting liquid left standstill 24 hours, get supernatant, being condensed into relative density is the thick paste of 1.35 (60-70 ℃), mixes with Common Coltsfoot Flower, drying is crushed to 80 orders, adds the sucrose of 25g, make granule, spray adds the 1.5g magnesium stearate with Oleum menthae, mixing, be pressed into 1000, sugar coating, promptly.
Its method of quality control comprises following several:
Differentiate:
(1) get 10 of this product, remove sugar-coat, porphyrize, the 25ml that adds diethyl ether makes dissolving, and supersound process 40 minutes is filtered, and filtrate is waved to 1.5ml, as need testing solution.Other Flos Farfarae control medicinal material 1g that withdraws the money shines medical material solution in pairs with legal system.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 25 μ l of above-mentioned two kinds of solution, respectively with same silica gel g thin-layer plate on, with normal hexane-ethyl acetate (4: 1) is developing solvent, launch, take out, dry, spray is with vanillin concentrated sulphuric acid test solution, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(2) get this product, remove sugar-coat, porphyrize takes by weighing 1g, adds 50 milliliters of dehydrated alcohol ultrasonic 10 minutes, filters, and the filtrate evaporate to dryness adds 1 milliliter of dissolving of dehydrated alcohol as test sample.Other gets Semen Oroxyli control medicinal material 2g, adds 50 milliliters of dehydrated alcohol ultrasonic 10 minutes, filters, and the filtrate evaporate to dryness adds 1 milliliter of dehydrated alcohol and dissolves medical material solution in contrast.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw above-mentioned sample solution 15 μ l, control medicinal material solution 5 μ l, respectively with same silica gel g thin-layer plate on, be developing solvent with cyclohexane extraction-ethyl acetate (9: 1), the expansion, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(3) sample thief is 10, removes sugar-coat, porphyrize, and 20 milliliters of chloroform-methanols (70: 30) soaked 3 hours, and ultrasonic 30 minutes, filter, evaporate to dryness is with 0.5 milliliter of dissolving of chloroform, as need testing solution.Other gets control medicinal material 2g Radix Ophiopogonis, shreds, with 20 milliliters of chloroform-methanols (70: 30), soaked 3 hours, and ultrasonic 30 minutes, filter, evaporate to dryness is with 0.5 milliliter of dissolving of chloroform, medical material solution in contrast.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw above-mentioned solution 10 μ l respectively, respectively with same silica gel g thin-layer plate on, with normal hexane-ethyl acetate (5: 1) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Check:
The n-butyl alcohol extractum takes by weighing this product, removes sugar-coat, porphyrize, get powder 2g, the accurate title, decide, the accurate methanol 50ml that adds, claim to decide weight, put in the water-bath reflux 1 hour, put cold, supply the weight that subtracts mistake with methanol, filter, get subsequent filtrate 25ml, put in the evaporating dish that is dried to constant weight, evaporate to dryness, residue add water 25ml, make dissolving, with water saturated n-butanol extraction 3 times, each 25ml, merge n-butyl alcohol liquid, put in the evaporating dish that is dried to constant weight evaporate to dryness, 105 ℃ of dryings 3 hours, in the dislocation exsiccator, placed 30 minutes, weight decided in accurate rapidly title, calculate, promptly.
Claims (3)
1. Chinese medicine composition for the treatment of chronic pharyngitis is characterized in that this Chinese medicine composition is made up of following weight portion crude drug:
Radix Scrophulariae 150～180 weight portion Radix Asteriss 120～150 weight portion Radix Asparagis 100～130 weight portions
Radix Arnebiae (Radix Lithospermi) 40～70 weight portion 50～80 weight portion system Flos Farfaraees Radix Ophiopogonis 40～70 weight portions
Semen Oroxyli 50～80 weight portion Radix Rehmanniae 50～80 weight portion Flos Loniceraes 200～230 weight portions
Rhizoma Belamcandae 120～150 weight portion Fructus Arctiis 40～70 weight portion Oleum menthae 0.4～0.6 weight portion.
2. treat the Chinese medicine composition of chronic pharyngitis according to claim 1, it is characterized in that this Chinese medicine composition is made up of following weight portion crude drug:
Radix Scrophulariae 170 weight portion Radix Asteriss 130 weight portion Radix Asparagis 120 weight portions
Radix Arnebiae (Radix Lithospermi) 50 weight portion 70 weight portion system Flos Farfaraees Radix Ophiopogonis 60 weight portions
Semen Oroxyli 70 weight portion Radix Rehmanniae 70 weight portion Flos Loniceraes 210 weight portions
Rhizoma Belamcandae 140 weight portion Fructus Arctiis 50 weight portion Oleum menthae 0.5 weight portion.
3. Chinese medicine composition according to claim 1, it is characterized in that this Chinese medicine composition routinely technology add adjuvant and make tablet, capsule, oral liquid, drop pill or granule; Described adjuvant comprises solvent, disintegrating agent, correctives, antiseptic, coloring agent, binding agent, lubricant, substrate.
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| CN101757555A (en) * | 2009-08-10 | 2010-06-30 | 黄山 | Capsule for treating pharyngitis |
| CN102397497B (en) * | 2011-11-26 | 2013-04-24 | 苏州派腾生物医药科技有限公司 | Method for preparing tablets for treating pharyngitis |
| CN102861226B (en) * | 2012-09-29 | 2014-06-18 | 曲延丽 | Traditional Chinese medicine for treating sphagitis |
| CN103800695A (en) * | 2014-03-07 | 2014-05-21 | 山东理工大学 | Traditional Chinese medicine composition for treating chronic pharyngitis |
| CN103800726A (en) * | 2014-03-07 | 2014-05-21 | 山东理工大学 | Traditional Chinese medicine composition for treating chronic pharyngitis |
| CN103800725A (en) * | 2014-03-07 | 2014-05-21 | 山东理工大学 | Chinese herbal medicine composition for treating chronic pharyngitis |
| CN104757477A (en) * | 2015-04-27 | 2015-07-08 | 宿州学院 | Chips suitable for being eaten by patients suffering from chronic pharyngitis |
| CN105106791B (en) * | 2015-09-16 | 2019-04-09 | 江苏七O七天然制药有限公司 | A kind of pharyngitis tea, preparation method and its identification method |
| CN106943560B (en) * | 2017-03-06 | 2018-07-24 | 广州上视医疗科技有限公司 | Traditional Chinese medicine composition for clearing lung and nourishing lung as well as preparation method and application thereof |
| CN107271598B (en) * | 2017-07-20 | 2018-12-04 | 青岛市食品药品检验研究院 | The construction method of Chinese patent drug Yanyan slice standard feature map and application |
| CN107496789A (en) * | 2017-07-27 | 2017-12-22 | 刘道鹏 | A kind for the treatment of pharyngitis capsule and preparation method thereof |
| CN108088715B (en) * | 2017-12-06 | 2021-03-16 | 广州科曼生物科技有限公司 | Moutan bark reference extract and preparation method and application thereof |
| CN110426486B (en) * | 2019-08-01 | 2021-08-17 | 正大青春宝药业有限公司 | Method for identifying Zhejiang ophiopogon root in traditional Chinese medicine preparation |
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| CN1739734A (en) * | 2005-09-06 | 2006-03-01 | 广州白云山和记黄埔中药有限公司 | Chinese medicine prepn for treating stomatitis and its prepn process |
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| 中华人民共和国卫生部药典委员会编.咽炎片.《卫生部颁药品标准（中药成方制剂第二册）》.1990, * |
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