CN102139040A - Quality control method of tablet capable of clearing lung and inhibiting fire - Google Patents
Quality control method of tablet capable of clearing lung and inhibiting fire Download PDFInfo
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Abstract
The invention relates to a quality control method of a tablet capable of clearing lung and inhibiting fire, which comprises the following steps of: adopting thin-layer chromatography to identify whether components such as gardenia, golden cypress, radix sophorae flavescentis and rheum officinale are contained in the formula of the tablet capable of clearing lung and inhibiting fire; taking baicalin as a contrast product; and adopting high efficiency liquid chromatography to measure the content of scutellaria baicalensis in the tablet capable of clearing lung and inhibiting fire. As an original quality standard does not have corresponding control standards, in the invention, thin-layer identification experiments are performed on the gardenia, golden cypress, radix sophorae flavescentis and rheum officinale, methods of screening materials characterized in good reproducibility, strong specificity, clear color development of spots, and easy judgment of results are contained in the standard; and based on the revised quality standard, the quality control of medicines is improved; therefore, the qualitative and quantitative detection of the medicines is more accurate, and the quality is easier to control.
Description
Technical field
The invention belongs to technical field of Chinese medicines, relate to the detection method of Chinese medicine, especially a kind of method of quality control of qingfei yihuo sheet.
Background technology
The main component and the content of qingfei yihuo sheet are as follows:
Radix Scutellariae 225g Fructus Gardeniae 129g Cortex Phellodendri 64g
Radix Et Rhizoma Rhei 193g Radix Sophorae Flavescentis 97g Radix Trichosanthis 129g
Rhizoma Anemarrhenae 97g Radix Platycodonis 129g Radix Peucedani 64g
Preparation method: above nine flavors, Radix Platycodonis, Radix Et Rhizoma Rhei powder are broken into fine powder; Fructus Gardeniae, the Rhizoma Anemarrhenae decoct with water secondary, and 2 hours for the first time, 1 hour for the second time, collecting decoction filtered, and filtrate is concentrated in right amount; Radix Peucedani, Radix Sophorae Flavescentis, Cortex Phellodendri, Radix Scutellariae extract three times with 60% alcohol heating reflux, and 3 hours for the first time, 2 hours for the second time, 1 hour for the third time; Radix Trichosanthis extracts three times with 25% alcohol heating reflux, and 3 hours for the first time, 2 hours for the second time, 1 hour for the third time, merge pure liquid, reclaim ethanol, be concentrated into an amount of.Merge above-mentioned water, pure concentrated solution, continue to be concentrated into thick paste, add powder and adjuvants such as Radix Platycodonis, mixing is made granule, drying; Concentrated solution after maybe will merging is spray dried to dried cream powder, adds powder and right amount of auxiliary materials such as Radix Platycodonis, and mixing is made granule.Be pressed into 1000, or the bag film-coat, that is, wherein: plain sheet: every heavy 0.6g, Film coated tablets: every heavy 0.61g.
Function with cure mainly: the lung heat clearing antitussive, pathogenic fire reducing promotes the production of body fluid.Be used for the cough due to lung-heat, accumulation and obstruction of sputum, laryngopharynx swelling and pain, mouth and nose are given birth to skin ulcer, tooth pain, dental root hemorrhage is hard and dry, yellowish or reddish urine.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, a kind of method of quality control of qingfei yihuo sheet that can the qualitative detection ingredient is provided, this method has that detection means is simple, testing result characteristic of accurate more.
The objective of the invention is to be achieved through the following technical solutions:
A kind of method of quality control of qingfei yihuo sheet, the step of its method is:
(1) is to product with jasminoidin, adopts the Fructus Gardeniae composition in the thin layer chromatography discriminating qingfei yihuo sheet;
(2) with the berberine hydrochloride be reference substance, adopt the Cortex Phellodendri composition in the thin layer chromatography discriminating qingfei yihuo sheet;
(3) with the matrine be reference substance, adopt the Radix Sophorae Flavescentis composition in the thin layer chromatography discriminating qingfei yihuo sheet;
(4) be that control medicinal material, chrysophanol, emodin are reference substance with the Radix Et Rhizoma Rhei, adopt thin layer chromatography to differentiate Radix Et Rhizoma Rhei composition in the qingfei yihuo sheet;
(5) with the baicalin be reference substance, adopt the Radix Scutellariae content in the high effective liquid chromatography for measuring qingfei yihuo sheet.
And described thin layer chromatography differentiates that the method for the Fructus Gardeniae in the prescription is:
1. the preparation of need testing solution: get qingfei yihuo sheet sample, porphyrize is got powder, adds 50% methanol, and supersound process filters, and filtrate is as need testing solution;
2. the preparation of reference substance solution: it is an amount of that other gets the jasminoidin reference substance, adds ethanol and make the solution that every 1ml contains 4mg, in contrast product solution;
3. thin layer chromatography and result: draw above-mentioned need testing solution, each 2-5 μ l of reference substance solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate: acetone: formic acid: water=5: 5: 1: 1 is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, 110 ℃ to be heated to speckle colour developing clear, inspect in the test sample chromatograph with reference substance chromatograph relevant position on whether show identical color speckle, determine whether contain the Fructus Gardeniae composition in the need testing solution.
And described thin layer chromatography differentiates that the method for the Cortex Phellodendri in the prescription is:
1. the preparation of need testing solution: get qingfei yihuo sheet sample, Film coated tablets is removed coating, and porphyrize is got powder 0.1g, adds diethyl ether, and jolting filters, and discards ether solution, and residue adds the methanol supersound process, filters, and filtrate is concentrated into 1ml, as need testing solution;
2. the preparation of reference substance solution: it is an amount of that other gets the berberine hydrochloride reference substance, adds methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution;
3. thin layer chromatography and result: draw above-mentioned need testing solution, each 2-5 μ l of reference substance solution, put respectively on same silica gel g thin-layer plate, with n-butyl alcohol: 36% acetic acid=7: 2 is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect, inspect in the test sample chromatograph with the corresponding position of reference substance chromatograph on whether show the fluorescence speckle of same color, determine whether contain the Fructus Gardeniae composition in the need testing solution.
And described thin layer chromatography differentiates that the method for the Radix Sophorae Flavescentis in the prescription is:
1. the preparation of need testing solution: get qingfei yihuo sheet sample respectively, Film coated tablets is removed coating, and porphyrize is got powder 6g, adds strong ammonia solution 2ml; Chloroform is placed and is spent the night, and filters, and filtrate evaporate to dryness, residue add chloroform makes dissolving, as need testing solution;
2. the preparation of reference substance solution: it is an amount of that other gets the matrine reference substance, adds methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution;
3. thin layer chromatography and result: draw above-mentioned need testing solution, reference substance solution, each 3-5 μ l of negative sample solution, put respectively on same silica gel g thin-layer plate, with toluene: acetone: ethyl acetate: strong ammonia solution=2: 3: 5: 0.2 is developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution, inspect in the test sample chromatograph with the corresponding position of reference substance chromatograph on whether show identical color speckle, determine whether contain the Radix Sophorae Flavescentis composition in the need testing solution.
And described thin layer chromatography differentiates that the method for the Radix Et Rhizoma Rhei in the prescription is:
1. the preparation of need testing solution: get qingfei yihuo sheet sample respectively, porphyrize is got powder 1g, adds methanol, and jolting is extracted, and filters, and filtrate is as need testing solution;
2. the preparation of control medicinal material solution: other gets the Radix Et Rhizoma Rhei control medicinal material, and porphyrize adds methanol 5ml, and jolting is extracted, and filters, and filtrate is medical material solution in contrast; The preparation of reference substance solution A: it is an amount of to get the chrysophanol reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast the product solution A; The preparation of reference substance solution B: it is an amount of to get the emodin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast the product solution B;
3. thin layer chromatography and result: inhale need testing solution 7-10 μ l, control medicinal material solution 4-6 μ l, reference substance A, each 2 μ l of B solution, put respectively on same silica gel g thin-layer plate, with petroleum ether: Ethyl formate: the upper solution of formic acid=15: 6: 2 is developing solvent, launch, take out, dry, place in the ammonia saturated with vapor expansion cylinder, inspect in the reference substance chromatograph with rhubarb medicinal material and the corresponding position of Radix Et Rhizoma Rhei reference substance chromatograph on whether show the speckle of same color, determine whether contain the Radix Et Rhizoma Rhei composition in the need testing solution.
And the method for the Radix Scutellariae content that described high performance liquid chromatogram detects is:
1. chromatograph and testing conditions: mobile phase: methanol: water: phosphoric acid=55: 45: 0.2, flow velocity: 1.0ml/min, column temperature: room temperature; Detect wavelength: 315nm, sample size: 10 μ l;
2. the preparation of reference substance solution: it is an amount of to get the baicalin reference substance, and accurate the title decides, and adds methanol and makes the solution that contains 0.1mg among every 1ml, promptly;
3. the preparation of need testing solution: get qingfei yihuo sheet sample, porphyrize, mixing, precision takes by weighing the 0.2g fine powder, puts in the tool plug conical flask, accurate 70% ethanol that adds, claim to decide weight, supersound process is put cold, claim to decide weight again, supply the weight that subtracts mistake with 70% ethanol, shake up, filter, get subsequent filtrate, promptly;
4. measure and the result: accurate respectively each the 10 μ l of reference substance solution, negative sample solution and need testing solution that draw, inject chromatograph of liquid, measure, that is, every heavy 0.6g of this product contains Radix Scutellariae and must not be less than 6.47mg in baicalin.
Advantage of the present invention and good effect are:
Owing to do not have the control corresponding standard in the proper mass standard, carried out the thin layer discrimination test of Fructus Gardeniae, Cortex Phellodendri, Radix Et Rhizoma Rhei, Radix Sophorae Flavescentis, Radix Platycodonis among the present invention, filter out that favorable reproducibility, specificity are strong, the speckle colour developing is clear, method that the result easily judges is included in the standard, revised quality standard, improved the quality control of medicine, make the qualitative and detection by quantitative of medicine more accurate, quality is more prone to control.
Description of drawings
The chromatogram that Fig. 1 differentiates for Fructus Gardeniae thin layer chromatography of the present invention is followed successively by from left to right: 1, sample 0512726,2, sample 0512724,3, sample 0601740,4, jasminoidin reference substance, 5, Fructus Gardeniae negative sample solution;
Fig. 2 is a Cortex Phellodendri thin layer chromatography identification color spectrogram of the present invention, is followed successively by from left to right: 1, sample 0512726,2, sample 0512724,3, sample 0601740,4, berberine hydrochloride reference substance, 5, Cortex Phellodendri negative sample solution;
Fig. 3 is a Radix Sophorae Flavescentis thin layer chromatography identification color spectrogram of the present invention, is followed successively by from left to right: 1, sample 0512726,2, sample 0512724,3, sample 0601740,4, matrine reference substance, 5, Radix Sophorae Flavescentis negative sample solution;
Fig. 4 is a Radix Et Rhizoma Rhei thin layer chromatography identification color spectrogram of the present invention, is followed successively by from left to right: 1, sample 0512726,2, sample 0512724,3, sample 0601740,4, Radix Et Rhizoma Rhei control medicinal material, 5, the chrysophanol reference substance, 6, emodin reference substance, 7, Radix Et Rhizoma Rhei negative sample solution;
Fig. 5 is a Radix Platycodonis thin layer chromatography identification color spectrogram of the present invention, is followed successively by from left to right: 1, sample 0512726,2, sample 0512724,3, sample 0601740,4, Radix Platycodonis control medicinal material, 5, Radix Platycodonis negative sample solution;
Fig. 6 is a baicalin reference substance solution chromatogram of the present invention;
Fig. 7 is a baicalin negative sample chromatogram of the present invention;
Fig. 8 is sample 0601740 chromatogram in the Radix Scutellariae detection of the present invention
Fig. 9 is sample 0512726 chromatogram in the Radix Scutellariae detection of the present invention;
Figure 10 is sample 0512724 chromatogram in the Radix Scutellariae detection of the present invention.
The specific embodiment
Below in conjunction with embodiment, the present invention is further described, and following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
A kind of method of quality control of qingfei yihuo sheet, the step of its method is:
(1) adopting thin layer chromatography, is reference substance with the jasminoidin, differentiates the Fructus Gardeniae in the prescription.
1. the preparation of need testing solution: get each 5 of qingfei yihuo sheet three batch samples, Film coated tablets is removed coating, and porphyrize is got powder art 1g, adds 50% methanol 10ml, and supersound process 40 minutes filters, and filtrate is as need testing solution.
2. the preparation of negative sample solution: by the prescription proportioning, get other medical materials except that Fructus Gardeniae,, make negative sample solution by above-mentioned need testing solution preparation method again by former medicine preparation technology film-making.
3. the preparation of reference substance solution: it is an amount of that other gets the jasminoidin reference substance, adds ethanol and make the solution that every 1ml contains 4mg, in contrast product solution.
4. thin layer chromatography and result: according to thin layer chromatography (" appendix VIB of Chinese pharmacopoeia version in 2005) test, draw above-mentioned need testing solution, reference substance solution, each 2-5 μ l of negative sample solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate: acetone: formic acid: water=5: 5: 1: 1 is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and 110 ℃ to be heated to the speckle colour developing clear, in the test sample chromatograph, with reference substance chromatograph relevant position on, show identical color speckle, negative sample solution is noiseless, the results are shown in Figure 1.
(2) adopting thin layer chromatography, is reference substance with the berberine hydrochloride, differentiates the Cortex Phellodendri in the prescription.
1. the preparation of need testing solution: get each 5 of qingfei yihuo sheet three batch samples, Film coated tablets is removed coating, and porphyrize is got powder 0.1g, 10ml adds diethyl ether, jolting 15 minutes filters, and discards ether solution, residue adds methanol 5ml supersound process 15 minutes, filter, filtrate is concentrated into 1ml, as need testing solution.
2. the preparation of negative sample solution: by the prescription proportioning, get other medical materials except that Cortex Phellodendri,, make negative sample solution by above-mentioned need testing solution preparation method again by former medicine preparation technology film-making.
3. the preparation of reference substance solution: it is an amount of that other gets the berberine hydrochloride reference substance, adds methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution.
4. thin layer chromatography and result: according to thin layer chromatography (" appendix VIB of Chinese pharmacopoeia version in 2005) test, draw above-mentioned need testing solution, reference substance solution, each 2-5 μ l of negative sample product solution, put respectively on same silica gel g thin-layer plate, with n-butyl alcohol: 36% acetic acid=7: 2 is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp 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, the results are shown in down Fig. 2.
Wherein: in the selection of developing solvent, in our the former method with benzene: ethyl acetate: isopropyl alcohol: methanol: strong ammonia solution=12: 6: 3: 3: 1, benzene: ethyl acetate: isopropyl alcohol: methanol: strong ammonia solution=12: 6: 3: 6: 2, benzene: ethyl acetate: isopropyl alcohol: methanol: strong ammonia solution=12: 6: 3: different development systems launched test 9: 3 etc., the result is with benzene: ethyl acetate: isopropyl alcohol: methanol: strong ammonia solution=12: 6: 3: 9: 3 expansion effect is best, because the toxicity of benzene is big, abandon using, use n-butyl alcohol instead: 36% acetic acid=7: 2 is that developing solvent launches, speckle is clear as a result, obviously, so to select this be the development system of Cortex Phellodendri.
(3) adopting thin layer chromatography, is reference substance with the matrine, differentiates the Radix Sophorae Flavescentis in the prescription.
1. the preparation of need testing solution: get each 15 of qingfei yihuo sheet three batch samples, Film coated tablets is removed coating, and porphyrize is got powder 6g, adds strong ammonia solution 2ml; Chloroform 30ml places and spends the night, and filters, and filtrate evaporate to dryness, residue add chloroform 2ml makes dissolving, as need testing solution.
2. the preparation of negative sample solution: by the prescription proportioning, get other medical materials except that Radix Sophorae Flavescentis,, make negative sample solution by above-mentioned need testing solution preparation method again by former medicine preparation technology film-making.
3. the preparation of reference substance solution: it is an amount of that other gets the matrine reference substance, adds methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution.
4. thin layer chromatography and result: according to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw above-mentioned need testing solution, reference substance solution, each 3-5 μ l of negative sample solution, put respectively on same silica gel g thin-layer plate, with toluene: acetone: ethyl acetate: strong ammonia solution=2: 3: 5: 0.2 is developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on show identical color speckle, negative sample solution is noiseless, the results are shown in Figure 3.
Wherein: the selection of developing solvent: we are with toluene: acetone: ethyl acetate: strong ammonia solution=2: 3: 4: 0.2, toluene: acetone: ethyl acetate: strong ammonia solution=2: 3: 5: different development system such as 0.2 launches test, the result is with toluene: acetone: ethyl acetate: strong ammonia solution=2: 3: 5: 0.2 expansion effect is best, speckle is clear, obvious, is the development system of Radix Sophorae Flavescentis so select this.
(4) adopting thin layer chromatography, is that control medicinal material, chrysophanol, emodin are reference substance with the Radix Et Rhizoma Rhei, differentiates the Radix Et Rhizoma Rhei in the prescription.
1. the preparation of need testing solution: get each 5 of qingfei yihuo sheet three batch samples, Film coated tablets is removed coating, and porphyrize is got powder art 1g, adds methanol 5ml, and jolting was extracted 30 minutes, filters, and filtrate is as need testing solution.
2. the preparation of negative sample solution: by the prescription proportioning, get other medical materials except that Radix Et Rhizoma Rhei,, make negative sample solution by above-mentioned need testing solution preparation method again by former medicine preparation technology film-making.
3. the preparation of control medicinal material solution: other gets Radix Et Rhizoma Rhei control medicinal material 0.3g, and porphyrize adds methanol 5ml, and jolting was extracted 30 minutes, filters, and filtrate is medical material solution in contrast; The preparation of reference substance solution A: it is an amount of to get the chrysophanol reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast the product solution A; The preparation of reference substance solution B: it is an amount of to get the emodin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast the product solution B.
4. thin layer chromatography and result: according to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, inhale need testing solution 7-10 μ l, control medicinal material solution 4-6 μ l, reference substance A, each 2 μ l of B solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (30-60 ℃): Ethyl formate: the upper solution of formic acid=15: 6: 2 is developing solvent, launch, take out, dry, place in the ammonia saturated with vapor expansion cylinder, in the reference substance chromatograph, with rhubarb medicinal material and the corresponding position of Radix Et Rhizoma Rhei reference substance chromatograph on show the speckle of same color, negative sample solution is noiseless, the results are shown in Figure 4.
Wherein: the selection of developing solvent: with petroleum ether (30-60 ℃): Ethyl formate: formic acid=15: 5: 1, petroleum ether (30-60 ℃): Ethyl formate: different development systems such as formic acid=15: 6: 2 launch test, the result is with petroleum ether (30-60 ℃): Ethyl formate: the expansion effect of the upper solution of formic acid=15: 6: 2 is best, speckle is clear, obvious, is the development system of Radix Et Rhizoma Rhei so select this.
(5) adopting thin layer chromatography, is contrast with the Radix Platycodonis control medicinal material, differentiates the Radix Platycodonis in the prescription.
Radix Platycodonis in the qingfei yihuo tablet recipe has been done the thin layer discriminating, because of result of the test undesirable, so the standard of excluding.
1. the preparation of need testing solution: get each 5 of qingfei yihuo sheet three batch samples, Film coated tablets is removed coating, porphyrize, get powder 1g, add 7% sulphuric acid ethanol: water=1: 3 mixed liquor 20ml, reflux 1 hour, put coldly, extract 2 times each 20ml with the chloroform jolting, combined chloroform liquid adds water 30ml washing and discards washing liquid, chloroform solution anhydrous sodium sulfate dehydration, filter, filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.
2. the preparation of negative sample solution: other gets the simulation qingfei yihuo sheet sample that lacks Radix Platycodonis, makes negative sample solution with former medicine preparation technology.
3. the preparation of control medicinal material solution: other gets Radix Platycodonis control medicinal material 1g, prepares control medicinal material solution by the need testing solution preparation method.
4. thin layer chromatography and result: according to thin layer chromatography (" appendix VIB of Chinese pharmacopoeia version in 2005) test, draw above-mentioned need testing solution, control medicinal material solution, each 4～6 μ l of negative need testing solution, put respectively on same silica gel g thin-layer plate, with chloroform: ether=1: 1 is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃.Result of the test: in test sample and the negative control liquid chromatography, with the corresponding position of control medicinal material chromatograph on, all show the speckle of same color.Be that the Radix Platycodonis negative sample has interference.Because of this method specificity is not strong,, the results are shown in Figure 5 so do not include in the standard.
(6) the Radix Scutellariae content of high performance liquid chromatogram detection
1. chromatograph and testing conditions: chromatographic column: the ODS-A of YMC company post (6.0mm * 150mm, 5 μ m); Mobile phase: methanol-water-phosphoric acid (55: 45: 0.2).Flow velocity: 1.0ml/min; Column temperature: room temperature.Detect wavelength: 315nm; Sample size: 10 μ l; Number of theoretical plate is not less than 2000 by baicalin.
2. the preparation of reference substance solution: it is an amount of to get the baicalin reference substance, and accurate the title decides, and adds methanol and makes the solution that contains 0.1mg among every 1ml, promptly.
3. the preparation of need testing solution: get 20 of qingfei yihuo sheet three batch samples, Film coated tablets is removed coating, porphyrize, mixing, precision take by weighing the 0.2g fine powder, put in the tool plug conical flask, the accurate 70% ethanol 25ml that adds claims to decide weight, supersound process 30 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with 70% ethanol, shake up, filter, get subsequent filtrate, promptly.
4. the preparation of negative sample solution is got the medical material of respectively distinguishing the flavor of except that Radix Scutellariae by prescription, makes sample by former medicine preparation technology, and 3. need testing solution preparation method set by step makes negative sample solution again.
5. measure and the result: accurate respectively each the 10 μ l of reference substance solution, negative sample solution and need testing solution that draw, inject chromatograph of liquid, measure, promptly, detect chromatogram and see Fig. 6, Fig. 7, Fig. 8, Fig. 9, Figure 10, every heavy 0.6g of this product contains Radix Scutellariae with baicalin (C
21H
18O
11) must not count and be less than 6.47mg.Computational methods are: Radix Scutellariae accounts for 19.96% of prescription total amount, in view of this product is that alcohol extraction is used as medicine, require (starch calculates by 60% rate of transform) according to Chinese Pharmacopoeia Commission, with reference to " content limit calculates under Radix Scutellariae item of Chinese pharmacopoeia version in 2005, and every of this product contains Radix Scutellariae with baicalin (C
21H
18O
11) meter, must not be less than 6.47mg.
Claims (6)
1. the method for quality control of a qingfei yihuo sheet, it is characterized in that: the step of its method is:
(1) is to product with jasminoidin, adopts the Fructus Gardeniae composition in the thin layer chromatography discriminating qingfei yihuo sheet;
(2) with the berberine hydrochloride be reference substance, adopt the Cortex Phellodendri composition in the thin layer chromatography discriminating qingfei yihuo sheet;
(3) with the matrine be reference substance, adopt the Radix Sophorae Flavescentis composition in the thin layer chromatography discriminating qingfei yihuo sheet;
(4) be that control medicinal material, chrysophanol, emodin are reference substance with the Radix Et Rhizoma Rhei, adopt thin layer chromatography to differentiate Radix Et Rhizoma Rhei composition in the qingfei yihuo sheet;
(5) with the baicalin be reference substance, adopt the Radix Scutellariae content in the high effective liquid chromatography for measuring qingfei yihuo sheet.
2. the method for quality control of qingfei yihuo sheet according to claim 1 is characterized in that: described thin layer chromatography differentiates that the method for the Fructus Gardeniae in the prescription is:
1. the preparation of need testing solution: get qingfei yihuo sheet sample, porphyrize is got powder, adds 50% methanol, and supersound process filters, and filtrate is as need testing solution;
2. the preparation of reference substance solution: it is an amount of that other gets the jasminoidin reference substance, adds ethanol and make the solution that every 1ml contains 4mg, in contrast product solution;
3. thin layer chromatography and result: draw above-mentioned need testing solution, each 2-5 μ l of reference substance solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate: acetone: formic acid: water=5: 5: 1: 1 is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, 110 ℃ to be heated to speckle colour developing clear, inspect in the test sample chromatograph with reference substance chromatograph relevant position on whether show identical color speckle, determine whether contain the Fructus Gardeniae composition in the need testing solution.
3. the method for quality control of qingfei yihuo sheet according to claim 1 is characterized in that: described thin layer chromatography differentiates that the method for the Cortex Phellodendri in the prescription is:
1. the preparation of need testing solution: get qingfei yihuo sheet sample, Film coated tablets is removed coating, and porphyrize is got powder 0.1g, adds diethyl ether, and jolting filters, and discards ether solution, and residue adds the methanol supersound process, filters, and filtrate is concentrated into 1ml, as need testing solution;
2. the preparation of reference substance solution: it is an amount of that other gets the berberine hydrochloride reference substance, adds methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution;
3. thin layer chromatography and result: draw above-mentioned need testing solution, each 2-5 μ l of reference substance solution, put respectively on same silica gel g thin-layer plate, with n-butyl alcohol: 36% acetic acid=7: 2 is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect, inspect in the test sample chromatograph with the corresponding position of reference substance chromatograph on whether show the fluorescence speckle of same color, determine whether contain the Fructus Gardeniae composition in the need testing solution.
4. the method for quality control of qingfei yihuo sheet according to claim 1 is characterized in that: described thin layer chromatography differentiates that the method for the Radix Sophorae Flavescentis in the prescription is:
1. the preparation of need testing solution: get qingfei yihuo sheet sample respectively, Film coated tablets is removed coating, and porphyrize is got powder 6g, adds strong ammonia solution 2ml; Chloroform is placed and is spent the night, and filters, and filtrate evaporate to dryness, residue add chloroform makes dissolving, as need testing solution;
2. the preparation of reference substance solution: it is an amount of that other gets the matrine reference substance, adds methanol and make the solution that every 1ml contains 0.5mg, in contrast product solution;
3. thin layer chromatography and result: draw above-mentioned need testing solution, reference substance solution, each 3-5 μ l of negative sample solution, put respectively on same silica gel g thin-layer plate, with toluene: acetone: ethyl acetate: strong ammonia solution=2: 3: 5: 0.2 is developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution, inspect in the test sample chromatograph with the corresponding position of reference substance chromatograph on whether show identical color speckle, determine whether contain the Radix Sophorae Flavescentis composition in the need testing solution.
5. the method for quality control of qingfei yihuo sheet according to claim 1 is characterized in that: described thin layer chromatography differentiates that the method for the Radix Et Rhizoma Rhei in the prescription is:
1. the preparation of need testing solution: get qingfei yihuo sheet sample respectively, porphyrize is got powder 1g, adds methanol, and jolting is extracted, and filters, and filtrate is as need testing solution;
2. the preparation of control medicinal material solution: other gets the Radix Et Rhizoma Rhei control medicinal material, and porphyrize adds methanol 5ml, and jolting is extracted, and filters, and filtrate is medical material solution in contrast; The preparation of reference substance solution A: it is an amount of to get the chrysophanol reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast the product solution A; The preparation of reference substance solution B: it is an amount of to get the emodin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast the product solution B;
3. thin layer chromatography and result: inhale need testing solution 7-10 μ l, control medicinal material solution 4-6 μ l, reference substance A, each 2 μ l of B solution, put respectively on same silica gel g thin-layer plate, with petroleum ether: Ethyl formate: the upper solution of formic acid=15: 6: 2 is developing solvent, launch, take out, dry, place in the ammonia saturated with vapor expansion cylinder, inspect in the reference substance chromatograph with rhubarb medicinal material and the corresponding position of Radix Et Rhizoma Rhei reference substance chromatograph on whether show the speckle of same color, determine whether contain the Radix Et Rhizoma Rhei composition in the need testing solution.
6. the method for quality control of qingfei yihuo sheet according to claim 1 is characterized in that: the method for the Radix Scutellariae content that described high performance liquid chromatogram detects is:
1. chromatograph and testing conditions: mobile phase: methanol: water: phosphoric acid=55: 45: 0.2, flow velocity: 1.0ml/min, column temperature: room temperature; Detect wavelength: 315nm, sample size: 10 μ l;
2. the preparation of reference substance solution: it is an amount of to get the baicalin reference substance, and accurate the title decides, and adds methanol and makes the solution that contains 0.1mg among every 1ml, promptly;
3. the preparation of need testing solution: get qingfei yihuo sheet sample, porphyrize, mixing, precision takes by weighing the 0.2g fine powder, puts in the tool plug conical flask, accurate 70% ethanol that adds, claim to decide weight, supersound process is put cold, claim to decide weight again, supply the weight that subtracts mistake with 70% ethanol, shake up, filter, get subsequent filtrate, promptly;
4. measure and the result: accurate respectively each the 10 μ l of reference substance solution, negative sample solution and need testing solution that draw, inject chromatograph of liquid, measure, that is, every heavy 0.6g of this product contains Radix Scutellariae and must not be less than 6.47mg in baicalin.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103134883A (en) * | 2011-11-28 | 2013-06-05 | 邯郸摩罗丹药业股份有限公司 | Medicine composition and detecting method of manufacturing agent of medicine composition |
| CN104374847A (en) * | 2014-07-31 | 2015-02-25 | 甘肃中天药业有限责任公司 | Detection method for rheum officinale medicinal material |
| CN110208420A (en) * | 2019-06-26 | 2019-09-06 | 贵州中医药大学 | A kind of quality determining method of the yellow bitter cream of compound |
| CN114848742A (en) * | 2022-03-30 | 2022-08-05 | 红云制药(昆明)有限公司 | Preparation method of lung-clearing and fire-inhibiting capsule |
| CN115607617A (en) * | 2022-05-27 | 2023-01-17 | 大理白族自治州中药制药有限公司 | Preparation method and detection method of lung-heat clearing and fire inhibiting tablet film-coated tablet |
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2010
- 2010-02-03 CN CN201010104906XA patent/CN102139040A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103134883A (en) * | 2011-11-28 | 2013-06-05 | 邯郸摩罗丹药业股份有限公司 | Medicine composition and detecting method of manufacturing agent of medicine composition |
| CN103134883B (en) * | 2011-11-28 | 2015-05-13 | 邯郸制药股份有限公司 | Medicine composition and detecting method of formula of medicine composition |
| CN104374847A (en) * | 2014-07-31 | 2015-02-25 | 甘肃中天药业有限责任公司 | Detection method for rheum officinale medicinal material |
| CN110208420A (en) * | 2019-06-26 | 2019-09-06 | 贵州中医药大学 | A kind of quality determining method of the yellow bitter cream of compound |
| CN114848742A (en) * | 2022-03-30 | 2022-08-05 | 红云制药(昆明)有限公司 | Preparation method of lung-clearing and fire-inhibiting capsule |
| CN114848742B (en) * | 2022-03-30 | 2024-03-15 | 红云制药(昆明)有限公司 | Preparation method of lung-heat clearing and fire suppressing capsule |
| CN115607617A (en) * | 2022-05-27 | 2023-01-17 | 大理白族自治州中药制药有限公司 | Preparation method and detection method of lung-heat clearing and fire inhibiting tablet film-coated tablet |
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Application publication date: 20110803 |