CN101524516A - Cholagogic pain-relieving capsule as well as preparation method and quality test and control method thereof - Google Patents
Cholagogic pain-relieving capsule as well as preparation method and quality test and control method thereof Download PDFInfo
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Abstract
The invention discloses a cholagogic pain-relieving capsule as well as a preparation method and a quality test and control method thereof. In the invention, the existing cholagogic pain-relieving tablets are improved significantly by adding prescription dosage, adopting reduced pressure low temperature concentration technology or reduced pressure low temperature concentration plus spray drying, reducing moisture in the extract to increase the medicament concentration, thus satisfying the requirement for the medicament preparation and optimizing the preparation technique. Meanwhile, the invention also provides a qualitative and quantitative method for product quality test and control, wherein TLC method is selected for authenticating five drugs, HPLC method is adopted for detecting the content of naringin, thus the cholagogic pain-relieving capsule is secure and effective and has controllable quality.
Description
Technical field
The present invention relates to a kind of medicine for the treatment of acute, chronic hepatitis, cholecystitis, more particularly, is to be the Chinese patent medicine of feedstock production with the Chinese herbal medicine.Simultaneously, the invention still further relates to the preparation method and the quality detection method of this medicine.
Background technology
As everyone knows, acute, chronic hepatitis, cholecystitis are a kind of commonly encountered diseases than refractory, and frequently-occurring disease is big to human health risk, must give active treatment.The medicine of integrative therapy is existing a variety of, and western medical treatment chronic hepatitis, cholecystitis are with antiinflammatory, infection, and enhance immunity etc. are main.And traditional Chinese medicine is much just abundant to the treatment means of acute and chronic hepatitis, cholecystitis, is mainly reflected in " dialectical executing controlled " and " symptomatic treatment in acute condition, relieving the primary symptom in a chronic case, giving consideration to both the incidental and fundamental " this two big treatment in principle.In acute hepatitis or chronic hepatitis, cholecystitis acute attack, and dialectical when being dampness-heat in the liver and gallbladder, with regard to clearing away heat-damp and promoting diuresis, the function of gallbladder promoting pain relieving, the person that has the depression of liver-QI is liver-smoothing, qi-regulating simultaneously just, but and in the also produce effects of function of gallbladder promoting pain relieving of regulating the flow of vital energy of the continuous usefulness of upper right abdomen dull pain usually, each side emphasizes particularly on different fields, and differs from one another.
Prescription of the present invention derives from ministry standard, the function of gallbladder promoting tablet for alleviating pain that the Chinese traditional patent formulation preparation is the 11st 90 pages, Radix Bupleuri (stir-fry) 60g, Radix Paeoniae Rubra 60g, Fructus Aurantii (parched) 60g, Radix Glycyrrhizae 30g Herba Artemisiae Scopariae 100g, Rhizoma Corydalis (stir-fry) 100g, Rhizoma Atractylodis 60g, Fructus Toosendan (stir-fry) 100g, Herba Agrimoniae 150g, Radix Isatidis 100g, Herba Taraxaci 150g, Rhizoma Curcumae Longae 100g, form by 12 flavor medical materials, be " Radix Bupleuri soothing liver-QI loose " (bright Zhang Jiebin " Jing Yue's complete work hypochondriac pain ") and " Sichuan Chinaberry Powder " (golden Liu Wansu " plain inquiring about disease machine gas should save one's life collection "), add Herba Artemisiae Scopariae, Herba Taraxaci, flavors such as Herba Agrimoniae form.The prescription that obtains of being harmonious is precise and appropriate and reliable, can play clearing heat secreting bile, the effect of regulating QI to relieve pain.Use it for acute and chronic hepatitis, cholecystitis belongs to dampness-heat in the liver and gallbladder person, disease is seen hypochondriac pain, jaundice, digestive disorders, asthenia, determined curative effects such as bitter taste.
The list marketing of function of gallbladder promoting tablet for alleviating pain is over more than 10 year, and reflection is pretty good, but the problem that exists also reveals gradually: (1) recipe quantity is little, causes dose big, and each 6, three times on the one, this has just influenced compliance that the patient takes medicine and to the selectivity of medicine; (2) in order to cover its bitterness, nude film has been carried out sugar coating, the molten laxity of medicine, this has just prolonged disintegration time, has influenced drug absorption; (3) method for making is limited to condition then, concentrates with room temperature, and long heat time heating time to extracting solution, the temperature height may cause ingredient to change; (4) supplementary product consumption is many; (5) chromogenic reaction is only arranged in the quality detection, specificity is not strong, restive drug quality.Many technical problems, anxious to be solved.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of improvement dosage form that can more effectively treat acute, chronic hepatitis, cholecystitis---function of gallbladder promoting acesodyne capsule is provided.
Another object of the present invention provides a kind of described capsular preparation method.
Further purpose of the present invention provides a kind of described capsular quality detection method.
Purpose of the present invention is achieved by following technical proposals.
* except as otherwise noted, the percent that is adopted among the present invention is quality amount percent.
A. the present invention makes described capsule raw materials of effective components medicine and forms and be by weight:
180～220 parts in 100～130 parts of Radix Bupleuri Chinensis (parched), 110～130 parts of Radix Paeoniae Rubra, 110～130 parts of Fructus Aurantii (parched), 50～70 parts in Radix Glycyrrhizae, 180～220 parts of Herba Artemisiae Scopariaes, 180～220 parts on Rhizoma Corydalis (parched) rope, 110～130 parts of Rhizoma Atractylodis, 180～220 parts of Fructus Toosendan (parched), 280～320 parts of Herba Agrimoniaes, 180～220 parts of Radix Isatidis, 280～320 parts of Herba Taraxacis and Rhizoma Curcumae Longae.
Be preferably: 200 parts in 120 parts of Radix Bupleuri Chinensis (parched), 120 parts of Radix Paeoniae Rubra, 120 parts of Fructus Aurantii (parched), 60 parts in Radix Glycyrrhizae, 200 parts of Herba Artemisiae Scopariaes, 200 parts on Rhizoma Corydalis (parched) rope, 120 parts of Rhizoma Atractylodis, 200 parts of Fructus Toosendan (parched), 300 parts of Herba Agrimoniaes, 200 parts of Radix Isatidis, 300 parts of Herba Taraxacis and Rhizoma Curcumae Longae.
Function of gallbladder promoting acesodyne capsule function of the present invention is clearing heat secreting bile, regulating QI to relieve pain with curing mainly.Be used for the hypochondriac pain due to the dampness-heat in the liver and gallbladder, jaundice (as acute and chronic hepatitis, cholecystitis).
The usage of function of gallbladder promoting acesodyne capsule and consumption are oral.One time 3,3 times on the one, every intragranular dress 0.4g.
B. the invention provides a kind of described capsular preparation method, this method adopts following steps:
(1) with described materials of weight proportions medicated powder broken be coarse powder, decoct with water three times, 2 hours for the first time, for the second time, three times each 1.5 hours, collecting decoction filtered;
(2) filtrate decompression is condensed into the thick paste of relative density 1.35～1.37 (60 ℃);
(3) the adding supplementary product starch is an amount of, and drying is pulverized, and adds an amount of starch and magnesium stearate again, and mixing is in incapsulating; Or behind the spice mixing, make granule earlier, and adding an amount of magnesium stearate after the drying again, mixing in incapsulating, promptly gets required capsule.
Use preparation technology of the present invention, add different conventional adjuvants respectively, promptly make oral formulations such as the identical granule of curative effect, soft capsule, drop pill, oral liquid, syrup.
C. function of gallbladder promoting acesodyne capsule of the present invention is with following its quality of qualitative method prosecution
(1) gets 10 of this product, take out content, put in the tool plug conical flask, add water 10ml, thixotropy is shaken diffusing, adds strong ammonia solution 0.5ml, ether 30ml, 20 seconds of jolting, supersound process is 30 minutes again, tells ether extracted liquid (water layer liquid is put in addition), evaporate to dryness, residue adds ethanol 0.5ml makes dissolving, as need testing solution.Other gets the tetrahydropalmatine reference substance, adds ethanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw need testing solution 8～15 μ l, reference substance solution 3～5 μ l put respectively on the silica gel g thin-layer plate of same usefulness 1% sodium hydroxide solution preparation, are developing solvent with toluene-acetone (9: 2), launch, take out, dry, put in the iodine cylinder and take out after about 3 minutes, wave the iodine that adsorbs on the most plate, inspect under the ultra-violet lamp (365nm).In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color; Negative noiseless.
(2) get the water layer liquid that ether extraction is crossed under discriminating (1) item, add hydrochloric acid furnishing acidity, add ethyl acetate 20ml, in 15 seconds of jolting, supersound process is 20 minutes again, tells acetic acid ethyl acetate extract (water layer liquid is put again), evaporate to dryness, residue add ethanol 0.5ml makes dissolving, as need testing solution.Other gets the naringin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution 8～15 μ l, reference substance solution 3～5 μ l put respectively on the silica gel g thin-layer plate of same usefulness 1% sodium hydroxide solution preparation, are developing solvent with ethyl acetate-methanol-water (100: 17: 13), launch, take out, dry, spray is with 5% aluminum chloride alcoholic solution, slightly be baked to driedly, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color, negative noiseless.
(3) get the water layer liquid that ethyl acetate extraction is crossed under discriminating (2) item, add water saturated n-butyl alcohol 20ml, in 15 seconds of jolting, supersound process is 20 minutes again, tell butanol extraction liquid, add ammonia solution 10ml, in 3 seconds of jolting, place and make layering, tell n-butyl alcohol liquid, evaporate to dryness, residue add ethanol 0.5ml makes dissolving, as need testing solution.Other gets Radix Bupleuri control medicinal material 0.3g, adds water 30ml, and little boiling 20 minutes boiled in heating, puts coldly, filters, and filtrate adds water saturated n-butyl alcohol 20ml shaking out, tells butanol extraction liquid, adds ammonia solution and shines medical material solution 0.5ml in pairs with legal system.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw need testing solution 8～15 μ l, control medicinal material solution 5～6 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with [the upper strata liquid of n-butyl alcohol-ethyl acetate-water (4: 1: 5)]-methanol (10: 1) is developing solvent, put in the vapour-saturated expansion cylinder of ammonia, launch, exhibition is apart from 12cm, take out, dry, spray the ethanol solution of sulfuric acid (1 → 10) with 1% paradime thylaminobenzaldehyde, it is clear to be baked to the speckle colour developing in 105 ℃.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color (and identical complexion changed), negative noiseless.
(4) get 8 of this product, take out content, put in the tool plug conical flask, add water 0.5ml, acetone 20ml firmly shakes diffusingly, and supersound process is 20 minutes again, tells acetone extract, and evaporate to dryness, residue add ethanol 0.5ml makes dissolving, as need testing solution.Extracting liquorice control medicinal material 0.2g shines medical material solution 1ml with control medicinal material under discriminating (3) item in pairs with legal system in addition.Get the peoniflorin reference substance again, add ethanol and make the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw need testing solution 8-15 μ l, each 3-5 μ l of control medicinal material and reference substance solution put respectively on the silica gel g thin-layer plate of same usefulness 1% sodium hydroxide solution preparation, with ethyl acetate-formic acid-glacial acetic acid-water (15: 1: 1: 2) be developing solvent, launch 12cm, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear to be baked to the speckle colour developing in 105 ℃, puts respectively under daylight and the ultra-violet lamp (365nm) and inspects.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color under the daylight respectively, under the ultra-violet lamp with the corresponding position of control medicinal material chromatograph on show the fluorescence speckle of same color, negative noiseless.
* the function of gallbladder promoting acesodyne capsule should meet relevant every regulation under an appendix IL of Chinese Pharmacopoeia version in 2005 the capsule item.
D. the function of gallbladder promoting acesodyne capsule is with following its quality of quantitative approach prosecution
(1) be filler according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D) mensuration chromatographic condition and system suitability test with octadecylsilane chemically bonded silica; With acetonitrile-0.1% phosphoric acid (17: 83) is mobile phase; The detection wavelength is 283nm; 40 ℃ of column temperatures.Number of theoretical plate calculates by the naringin peak should be not less than 4000.
(2) preparation of reference substance solution---precision takes by weighing at 110 ℃ of naringin reference substances that are dried to constant weight an amount of, adds methanol and makes the solution that every 1ml contains 60 μ g, promptly.
The content under this product content uniformity item is got in the preparation of need testing solution, and mixing is got 0.5g, and accurate the title decides, put in the tool plug conical flask, the accurate mobile phase 25ml that adds, close plug claims to decide weight, shake diffusingly, supersound process 10 minutes is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with mobile phase, incline to and put in right amount in the centrifuge tube, jump a queue, centrifugal 20 minutes (4000 commentaries on classics/min), get supernatant and filter, get subsequent filtrate, promptly with 0.45 μ m microporous filter membrane.
(3) algoscopy---accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly.Every of this product contains Fructus Aurantii with naringin (C
27H
32O
14) meter, must not be less than 1.0mg.
Compared with prior art, the present invention has following outstanding advantage:
1. at above-mentioned deficiency, in that to guarantee that pharmic function cures mainly constant, safely and effectively under the prerequisite, make tablet into capsule (belonging to new Chinese medicine 8 classes in the medicine registration management way), capsule of the present invention has the bitterness that can cover medicine and smells flavor, can have shades of colour, and all right lettering is as a means of difference, and attractive in appearance, be beneficial to take, advantage that compliance is good, easy to carry.
2. bioavailability of medicament height, capsule needs to add binding agent and pressure unlike tablet, pill in the preparation, so in intestines and stomach, decompose fast, good absorbing.Improve medicine stability, guarantee that medicine is not subjected to the effect of dampness and airborne oxygen, light.
3. the increase prescribed dose prepares the decompression cryoconcentration technology that adopted, or decompression cryoconcentration+spray drying, reduces the moisture in the extract, has improved drug level, has satisfied the pharmaceutical preparation requirement, ensures the quality of products.
4. each dose is kept to 3, has improved the selectivity of patient's medication and the compliance of taking.
5. set up more perfect quality control index and detection method, differentiated 5 kinds of medical materials such as Rhizoma Corydalis, Fructus Aurantii, Radix Bupleuri, Radix Glycyrrhizae, Radix Paeoniae Rubra with the TLC method qualitatively.Must analyze naringin content with the HPLC standard measure.Press under 2005 editions one appendix I L of the Chinese Pharmacopoeia capsule item and to check, (Pb＜10ppm) presses 2005 editions one appendix IXF arsenic of Chinese Pharmacopoeia salt inspection technique survey arsenic (As＜2ppm) press 2005 editions one appendix IXE heavy metal of Chinese Pharmacopoeia inspection technique check weighing metal.
6. through a series of improvement, the function of gallbladder promoting acesodyne capsule occurs with brand-new looks, the dosage form novelty, and preparation method advanced person, quality controllable, curative effect is reliable.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
The specific embodiment
By specific embodiment given below and typical Application Example, can further be well understood to the present invention.But they are not the qualification to protection domain of the present invention.
Embodiment 1
Making capsule raw materials of effective components medicine of the present invention consists of: Radix Bupleuri (stir-fry) 120g, Radix Paeoniae Rubra 120g, Fructus Aurantii (parched) 120g, Radix Glycyrrhizae 60g Herba Artemisiae Scopariae 200g, Rhizoma Corydalis (stir-fry) 200g, Rhizoma Atractylodis 120g, Fructus Toosendan (stir-fry) 200g, Herba Agrimoniae 300g, Radix Isatidis 200g, Herba Taraxaci 300g and Rhizoma Curcumae Longae 200g.Be crushed into coarse powder, decoct with water three times, 2 hours for the first time, three times each 1.5 hours for the second time,, collecting decoction filters, and filtrate decompression is condensed into the thick paste of relative density 1.35～1.37 (60 ℃), it is an amount of to add supplementary product starch, drying is pulverized, and adds an amount of starch and magnesium stearate again, mixing is in incapsulating; Or behind the spice mixing, make granule before not adding magnesium stearate, and dry back adds an amount of magnesium stearate, and mixing in incapsulating, is made 1000, promptly gets required function of gallbladder promoting acesodyne capsule.
Embodiment 2
The optimization method that decocting boils technology is: the prescription medical material amount (2140g) of getting system 1000 capsules, the multiple of according to the form below adds water, the number of times (three times) that each decocts, time (2 hours, 1.5 hours, 1.5 hours) is all identical, and being adjusted to the water quantities that contains of each time gained dry extract about the samely, test data sees Table 1.
Table 1.
The content assaying method of the naringin in the table 1 is to use the HPLC method.Table 1 shows, is index with the total solid, adds that water more more to get dry extract manyly more, and as being index with the final extraction total amount of naringin, it is just passable to add 8 times～10 times amounts of water, and the extraction of 8 times, 10 times and 12 times water yields difference as a result is very not big.
Embodiment 3
---the test data that middle trial production is three batches
* press recipe quantity and amplify 10 times, and produce three batches of products by above-mentioned preparation process, test data sees Table.
| Lot number | 20040901 | 20040902 | 20040903 |
| The total inventory of medical material (kg) | 21.4 | 21.4 | 21.4 |
| Decocting decoct medicinal herbs material amount (kg) | 21.4 | 21.4 | 21.4 |
| Extractum must be measured (kg) | 4.15 | 4.12 | 4.16 |
| Extractum relative density (80 ℃) | 1.36 | 1.37 | 1.36 |
| Add amount of starch (Kg) earlier | 0.8 | 0.8 | 0.8 |
| Cream, powder are dried back weight (kg) | 3.70 | 3.72 | 3.69 |
| The cream powder is pulverized back weight (kg) | 3.63 | 3.65 | 3.61 |
| After add amount of starch (kg) | 0.3 | 0.3 | 0.3 |
| Add magnesium stearate (kg) | 0.1 | 0.1 | 0.1 |
| Make qualified spice (kg) | 4.03 | 4.05 | 4.01 |
| Capsule charge (grain) | 9600 | 9800 | 9500 |
| Designing capacity (grain) | 10000 | 10000 | 10000 |
| Yield rate (%) | 96 | 98 | 95 |
More than the three batches of finished products through check: character, discriminating, moisture, disintegration, weight differential, assay and microbial check all qualified (according to from intend the quality standard draft and " pertinent regulations of Chinese pharmacopoeia appendix).
Embodiment 4
The discriminating of Rhizoma Corydalis.Get 10 of this product, take out content, put in the tool plug conical flask, add water 10ml, thixotropy is shaken diffusing, adds strong ammonia solution 0.5ml, ether 30ml, 20 seconds of jolting, supersound process is 30 minutes again, tells ether extracted liquid (water layer liquid is put in addition), evaporate to dryness, residue adds ethanol 0.5ml makes dissolving, as need testing solution.Other gets the tetrahydropalmatine reference substance, adds ethanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution 8～15 μ l, reference substance solution 3～5 μ l put respectively on the silica gel g thin-layer plate of same usefulness 1% sodium hydroxide solution preparation, are developing solvent with toluene-acetone (9: 2), launch, take out, dry, put in the iodine cylinder and take out after about 3 minutes, wave the iodine that adsorbs on the most plate, inspect under the ultra-violet lamp (365nm).In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color, negative noiseless.
Embodiment 5
The discriminating of Fructus Aurantii.Get the water layer liquid that ether extraction is crossed under discriminating (Rhizoma Corydalis) item, add hydrochloric acid furnishing acidity, add ethyl acetate 20ml, in 15 seconds of jolting, supersound process is 20 minutes again, tells acetic acid ethyl acetate extract (water layer liquid is put again), evaporate to dryness, residue add ethanol 0.5ml makes dissolving, as need testing solution.Other gets the naringin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution 8～15 μ l, reference substance solution 3～5 μ l put respectively on the silica gel g thin-layer plate of same usefulness 1% sodium hydroxide solution preparation, are developing solvent with ethyl acetate-methanol-water (100: 17: 13), launch, take out, dry, spray is with 5% aluminum chloride alcoholic solution, slightly be baked to driedly, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color, negative noiseless.
Embodiment 6
The discriminating of Radix Bupleuri.Get the water layer liquid that ethyl acetate extraction is crossed under discriminating (Fructus Aurantii) item, add water saturated n-butyl alcohol 20ml, in 15 seconds of jolting, supersound process is 20 minutes again, tell butanol extraction liquid, add ammonia solution 10ml, in 3 seconds of jolting, place and make layering, tell n-butyl alcohol liquid, evaporate to dryness, residue add ethanol 0.5ml makes dissolving, as need testing solution.Other gets Radix Bupleuri control medicinal material 0.3g, adds water 30ml, and little boiling 20 minutes boiled in heating, puts coldly, filters, and filtrate adds water saturated n-butyl alcohol 20ml shaking out, tells butanol extraction liquid, adds ammonia solution and shines medical material solution 0.5ml in pairs with legal system.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw need testing solution 8～15 μ l, control medicinal material solution 5～6 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with [the upper strata liquid of n-butyl alcohol-ethyl acetate-water (4: 1: 5)]-methanol (10: 1) is developing solvent, put in the vapour-saturated expansion cylinder of ammonia, launch, exhibition is apart from 12cm, take out, dry, spray the ethanol solution of sulfuric acid (1 → 10) with the l% paradime thylaminobenzaldehyde, it is clear to be baked to the speckle colour developing in 105 ℃.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color (and identical complexion changed), negative noiseless.
Embodiment 7
The discriminating of Radix Glycyrrhizae and Radix Paeoniae Rubra.Get 8 of this product, take out content, put in the tool plug conical flask, add water 0.5ml, acetone 20ml firmly shakes diffusingly, and supersound process is 20 minutes again, tells acetone extract, and evaporate to dryness, residue add ethanol 0.5ml makes dissolving, as need testing solution.Extracting liquorice control medicinal material 0.2g shines medical material solution 1ml with control medicinal material under discriminating (Radix Bupleuri) item in pairs with legal system in addition.Get the peoniflorin reference substance again, add ethanol and make the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw need testing solution 8-15 μ l, each 3-5 μ l of control medicinal material and reference substance solution put respectively on the silica gel g thin-layer plate of same usefulness 1% sodium hydroxide solution preparation, with ethyl acetate-formic acid-glacial acetic acid-water (15: 1: 1: 2) be developing solvent, launch 12cm, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear to be baked to the speckle colour developing in 105 ℃, puts respectively under daylight and the ultra-violet lamp (365nm) and inspects.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color under the daylight respectively, under the ultra-violet lamp with the corresponding position of control medicinal material chromatograph on show the fluorescence speckle of same color, negative noiseless.
Embodiment 8
The assay of naringin.Measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; With acetonitrile-0.1% phosphoric acid (17: 83) is mobile phase; The detection wavelength is 283nm; 40 ℃ of column temperatures.Number of theoretical plate calculates by the naringin peak should be not less than 4000.The preparation precision of reference substance solution takes by weighing at 110 ℃ of naringin reference substances that are dried to constant weight an amount of, adds methanol and makes the solution that every 1ml contains 60 μ g, promptly.
---the preparation of need testing solution.Get the content under this product content uniformity item, mixing is got 0.5g, and accurate the title decides, put in the tool plug conical flask, the accurate mobile phase 25ml that adds, close plug claims to decide weight, shake diffusingly, supersound process 10 minutes is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with mobile phase, incline to and put in right amount in the centrifuge tube, jump a queue, centrifugal 20 minutes (4000 commentaries on classics/min), get supernatant and filter, get subsequent filtrate, promptly with microporous filter membrane (0.45 μ m).
---algoscopy.Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly.
Every of this product contains Fructus Aurantii with naringin (C
27H
32O
14) meter, must not be less than 1.0mg.The assay of ten batch samples the results are shown in Table.
Embodiment 9
Above-mentioned 12 flavor crude drug, pulverize to coarse powder, decoct with water three times, 2 hours for the first time, three times each 1.5 hours for the second time,, collecting decoction filters, and filtrate decompression is condensed into the thick paste of relative density 1.35～1.37 (60 ℃), add an amount of dextrin, Icing Sugar, mixing, granulation are made 333 bags, promptly get required granule,
Embodiment 10
Above-mentioned 12 flavor crude drug are pulverized and are coarse powder, decoct with water three times, 2 hours for the first time, for the second time, three times each 1.5 hours, collecting decoction filters, filtrate decompression is condensed into the thick paste of relative density 1.35～1.37 (60 ℃), add adjuvant polyvinyl alcohol 6000, or Macrogol 4000, medicine: substrate=(1: the 1-4) mixing of heating, make with dropping-pill machine, promptly.
Embodiment 11
Above-mentioned 12 flavor crude drug are pulverized and are coarse powder, decoct with water three times, 2 hours for the first time, for the second time, three times each 1.5 hours, collecting decoction filters, filtrate decompression is condensed into the clear paste of relative density 1.08 (60 ℃), it is an amount of to add syrup, dilute with water, mixing, make 3000ml, promptly get required syrup.
Embodiment 12
Above-mentioned 12 flavor crude drug are pulverized and are coarse powder, decoct with water three times, 2 hours for the first time, for the second time, three times each 1.5 hours, collecting decoction, filter, filtrate decompression is condensed into the clear paste of relative density 1.08 (60 ℃), and the adding correctives is an amount of, adds the dilution of 2000ml water, leave standstill diel, filter, add water to 3000ml again, promptly get required oral liquid.
Embodiment 13
Above-mentioned 12 flavor crude drug are pulverized and are coarse powder, decoct with water three times, 2 hours for the first time, for the second time, three times each 1.5 hours, collecting decoction filters, filtrate decompression is condensed into the thick paste of relative density 1.35～1.37 (60 ℃), add oils and fats, right amount of auxiliary materials, mixing places on the machine of automatic rotation Zhanang, be sealed in the soft capsule material with pressing, promptly get required soft capsule.
Claims (5)
1. function of gallbladder promoting acesodyne capsule, it is characterized in that the composition of making this capsule raw materials of effective components medicine is by weight: 100～130 parts of Radix Bupleuri Chinensis (parched), 110～130 parts of Radix Paeoniae Rubra, fry 180～220 parts in 110～130 parts of trifoliate oranges, 50～70 parts in Radix Glycyrrhizae, 180～220 parts of Herba Artemisiae Scopariaes, 180～220 parts of Rhizoma Corydalis (parched), 110～130 parts of Rhizoma Atractylodis, 180～220 parts of Fructus Toosendan (parched), 280～320 parts of Herba Agrimoniaes, 180～220 parts of Radix Isatidis, 280～320 parts of Herba Taraxacis and Rhizoma Curcumae Longae.
2. capsule according to claim 1, it is characterized in that the composition of making this capsule raw materials of effective components medicine is by weight: 200 parts in 120 parts of Radix Bupleuri Chinensis (parched), 120 parts of Radix Paeoniae Rubra, 120 parts of Fructus Aurantii (parched), 60 parts in Radix Glycyrrhizae, 200 parts of Herba Artemisiae Scopariaes, 200 parts on Rhizoma Corydalis (parched) rope, 120 parts of Rhizoma Atractylodis, 200 parts of Fructus Toosendan (parched), 300 parts of Herba Agrimoniaes, 200 parts of Radix Isatidis, 300 parts of Herba Taraxacis and Rhizoma Curcumae Longae.
3. the preparation method of a function of gallbladder promoting acesodyne capsule is characterized in that, this method adopts following steps:
(1) with described materials of weight proportions medicated powder broken be coarse powder, decoct with water three times, 2 hours for the first time, for the second time, three times each 1.5 hours, collecting decoction filtered;
(2) filtrate becomes the thick paste of relative density 1.35～1.37 at 60 ℃ of following concentrating under reduced pressure;
(3) the adding supplementary product starch is an amount of, and drying is pulverized, and adds an amount of starch and magnesium stearate again, and mixing is in incapsulating; Or behind the spice mixing, make granule earlier, and adding an amount of magnesium stearate after the drying again, mixing in incapsulating, promptly gets required capsule.
4. the qualitative detecting and control method of claim 1 or 2 described function of gallbladder promoting acesodyne capsule quality is characterized in that adopting following steps:
(1) gets 10 of this product, take out content, put in the tool plug conical flask, add water 10ml, thixotropy is shaken diffusing, adds strong ammonia solution 0.5ml, ether 30ml, in 20 seconds of jolting, supersound process is 30 minutes again, tells ether extracted liquid, water layer liquid is put in addition, evaporate to dryness, residue add ethanol 0.5ml makes dissolving, as need testing solution; Other gets the plain reference substance of court of a feudal ruler Rhizoma Corydalis second, adds ethanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography, draw need testing solution 8～15 μ l, reference substance solution 3～5 μ l put respectively on the silica gel g thin-layer plate of same usefulness 1% sodium hydroxide solution preparation, and with toluene: acetone=9: 2 is developing solvent, launch, take out, dry, put in the iodine cylinder and take out after about 3 minutes, wave the iodine that adsorbs on the most plate, inspect under the ultra-violet lamp 365nm; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color; Negative noiseless.
(2) get and differentiate and to add hydrochloric acid furnishing acidity by 1 the water layer liquid that following ether extraction is crossed, add ethyl acetate 20ml, 15 seconds of jolting, supersound process is 20 minutes again, tells acetic acid ethyl acetate extract, and water layer liquid is put again, evaporate to dryness, residue add ethanol 0.5ml makes dissolving, as need testing solution; Other gets the naringin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography, draw need testing solution 8～15 μ l, reference substance solution 3～5 μ l put respectively on the silica gel g thin-layer plate of same usefulness 1% sodium hydroxide solution preparation, and with ethyl acetate: methanol: water=100: 17: 13 is developing solvent, launch, take out, dry, spray is with 5% aluminum chloride alcoholic solution, slightly baking as for, put under the ultra-violet lamp 365nm and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color; Negative noiseless.
(3) get 2 water layer liquid that following ethyl acetate extraction is crossed of discriminating, add water saturated n-butyl alcohol 20ml, in 15 seconds of jolting, supersound process is 20 minutes again, tell butanol extraction liquid, add ammonia solution 10ml, in 3 seconds of jolting, place and make layering, tell n-butyl alcohol liquid, evaporate to dryness, residue add ethanol 0.5ml makes dissolving, as need testing solution; Other gets Radix Bupleuri control medicinal material 0.3g, adds water 30ml, and little boiling 20 minutes boiled in heating, puts coldly, filters, and filtrate adds water saturated n-butyl alcohol 20ml shaking out, tells butanol extraction liquid, adds ammonia solution and shines medical material solution 0.5ml in pairs with legal system; Test according to thin layer chromatography, draw need testing solution 8～15 μ l, control medicinal material solution 5～6 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with n-butyl alcohol: ethyl acetate: the upper strata liquid of water=4: 1: 5: methanol=10: 1 is developing solvent, puts in the vapour-saturated expansion cylinder of ammonia, launch, the ethanol solution of sulfuric acid 1 → 10 with 1% paradime thylaminobenzaldehyde is taken out, dries, sprayed to exhibition apart from 12cm, and it is clear to be baked to the speckle colour developing in 105 ℃.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color and identical complexion changed; Negative noiseless.
(4) get 8 of this product, take out content, put in the tool plug conical flask, add water 0.5ml, acetone 20ml firmly shakes diffusingly, and supersound process is 20 minutes again, tells acetone extract, and evaporate to dryness, residue add ethanol 0.5ml makes dissolving, as need testing solution; Extracting liquorice control medicinal material 0.2g shines medical material solution 1ml with 3 following control medicinal materials of discriminating in pairs with legal system in addition; Get the peoniflorin reference substance again, add ethanol and make the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw need testing solution 8-15 μ l, each 3-5 μ l of control medicinal material and reference substance solution puts respectively on the silica gel g thin-layer plate of same usefulness 1% sodium hydroxide solution preparation, and with ethyl acetate: formic acid: glacial acetic acid: water=15: 1: 1: 2 is developing solvent, launch 12cm, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear to be baked to the speckle colour developing in 105 ℃, puts respectively under daylight and the ultra-violet lamp 365nm and inspects; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color under the daylight respectively, under the ultra-violet lamp with the corresponding position of control medicinal material chromatograph on show the fluorescence speckle of same color; Negative noiseless.
The function of gallbladder promoting acesodyne capsule should meet relevant every regulation under an appendix IL of Chinese Pharmacopoeia version in 2005 the capsule item.
5. the quantitative detecting and control method of claim 1 or 2 described function of gallbladder promoting acesodyne capsule quality is characterized in that adopting following steps:
(1) according to high effective liquid chromatography for measuring---chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; With acetonitrile: 0.1% phosphoric acid=17: 83 is mobile phase; The detection wavelength is 283nm; 40 ℃ of column temperatures; Number of theoretical plate calculates by the naringin peak should be not less than 4000;
(2) preparation of reference substance solution---precision takes by weighing at 110 ℃ of naringin reference substances that are dried to constant weight an amount of, adds methanol and makes the solution that every 1ml contains 60 μ g, promptly;
The content under this product content uniformity item is got in the preparation of need testing solution, and mixing is got 0.5g, and accurate the title decides, put in the tool plug conical flask, the accurate mobile phase 25ml that adds, close plug claims to decide weight, shake diffusingly, supersound process 10 minutes is put coldly, claims to decide weight again, supply the weight that subtracts mistake with mobile phase, shake up, incline to and put in right amount in the centrifuge tube, jump a queue, centrifugal 20 minutes, 4000 commentaries on classics/min, get supernatant and filter, get subsequent filtrate, promptly with 0.45 μ m microporous filter membrane;
(3) algoscopy---accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; Every of this product contains Fructus Aurantii in naringin, must not be less than 1.0mg.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104840629A (en) * | 2015-05-18 | 2015-08-19 | 新希望六和饲料股份有限公司 | Drug composition for treating cat jaundice and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104840629A (en) * | 2015-05-18 | 2015-08-19 | 新希望六和饲料股份有限公司 | Drug composition for treating cat jaundice and preparation method thereof |
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Application publication date: 20090909 |