CN100432670C - Method for inspecting Chinese-medicinal preparation Kaiyinwan - Google Patents

Method for inspecting Chinese-medicinal preparation Kaiyinwan Download PDF

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CN100432670C
CN100432670C CNB2007100176210A CN200710017621A CN100432670C CN 100432670 C CN100432670 C CN 100432670C CN B2007100176210 A CNB2007100176210 A CN B2007100176210A CN 200710017621 A CN200710017621 A CN 200710017621A CN 100432670 C CN100432670 C CN 100432670C
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paeoniflorin
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methyl alcohol
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CN101029890A (en
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黄小华
付彬
张�浩
雒西萍
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BEILIN PHARMACEUTICAL Co Ltd XI'AN
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BEILIN PHARMACEUTICAL Co Ltd XI'AN
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Abstract

A method for detecting quality of Chinese medicine preparation for curing laryngeal disease utilizes proper solvent and optimum prepared test sample to carry out effective qualitative analysis on radix scutellariae glucoside and great burdock glucoside. The method for detecting content of Chinese herbaceous peony glucoside is also disclosed.

Description

A kind of quality determining method of Chinese medicine preparation Kaiyinwan ball
One, technical field:
The present invention relates to a kind of quality determining method, particularly relate to a kind of quality determining method of Chinese medicine preparation Kaiyinwan ball, belong to the field of Chinese medicines.
Two, background technology:
Honeysuckle, capsule of weeping forsythia dispelling wind and heat from the body are clearing heat and detoxicating in the Chinese traditional compound medicine Kaiyinwan ball side made from honeysuckle, the capsule of weeping forsythia, Radix Isatidis, the root of large-flowered skullcap etc., and the detumescence relieve sore throat is monarch drug in a prescription.Radix Isatidis, root of large-flowered skullcap clearing heat-fire, removing pattogenic heat from the blood and toxic material from the body, detumescence relieve sore throat; Mulberry leaf, chrysanthemum, the sterculia seed, great burdock achene, cicada slough wind and heat dispersing, the detoxifcation of reducing phlegm, detumescence relieve sore throat; The root of purple-flowered peucedanum, stiff silkworm, semen armeniacae amarae clearing heat and eliminating phlegm, the dissipating bind relieve sore throat, this ten flavor is ministerial drug altogether.The rhizoma alismatis dampness removing is eliminating evil, and evil poison is gone out from urine; The dehematize heat of branch of radix scrophulariae, the radix paeoniae rubrathe, removing pattogenic heat from the blood and toxic material from the body, mass dissipating and swelling eliminating; The Oroxylum indicum moistening lung and nourishing throat, it is mute to open musicotherapy, is treatment pharyngolaryngitis key medicine, and four medicines share and are adjutant.All medicines share, play altogether clearing heat and detoxicating, the effect of dispelling wind relieve sore throat.Be used for the abscess of throat due to the evil poison of wind-heat, hoarseness; Acpuei pharyngitis, laryngitis are seen above-mentioned patient, and effect is obvious.Yet the Chinese medicinal ingredients more complicated contains many unknown compositions.Can effectively control the product quality of treatment eye illness myopia and asthenopic Chinese medicine preparation at present, detection method that can be easy to operate is not also reported again.For promoting the Chinese medicine preparation modernization, Chinese medicine preparation research quality determining method is necessary.
Three, summary of the invention:
The object of the present invention is to provide and a kind ofly can effectively control Chinese medicine preparation Kaiyinwan ball quality, the quality determining method that accuracy is high.
The quality determining method of a kind of Chinese traditional compound medicine Kaiyinwan ball of the present invention, with honeysuckle, the capsule of weeping forsythia, radix scrophulariae, Radix Isatidis, the radix paeoniae rubrathe, the root of large-flowered skullcap, mulberry leaf, chrysanthemum, the root of purple-flowered peucedanum, semen armeniacae amarae (fire is single), great burdock achene, rhizoma alismatis, the sterculia seed, stiff silkworm (bran stir-fry), cicada slough, Oroxylum indicum ten Six-element medicines, be ground into fine powder, sieve mixing; Every 100g powder adds refined honey 35~50g and an amount of water, pill, and drying is used the activated charcoal dressing, makes water-honeyed pill; Or add refined honey 110g~130g and make big honeyed pills, its detection method may further comprise the steps:
(1) gets this product water-honeyed pill 5g, grind; Or get big honeyed pills 8g, and shred, add zeyssatite 4g, grind well; Add methyl alcohol 40ml, sonicated 30 minutes filters, and filtrate evaporate to dryness, residue add water 20ml makes dissolving, transfers pH value to being about 2 with watery hydrochloric acid, extracts 2 times with the ethyl acetate jolting, and each 20ml merges extract, evaporate to dryness; Residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets the scutelloside reference substance, adds methyl alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin-layered chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with 5: 3: 1: ethyl acetate-butanone of 1-formic acid-aqueous solution was a developping agent, launch, take out, dry, spray is with 2% ferric trichloride ethanolic solution; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(2) get this product water-honeyed pill 5g, grind; Or get big honeyed pills 8g, and shred, add zeyssatite 4g, grind well; The mixed solution 40ml that adds ethyl acetate-methyl alcohol of 2: 1, sonicated 20 minutes filters, and filtrate evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution; Other gets burdock glycosides reference substance, adds methyl alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin-layered chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with methenyl choloride-methanol-waters of 40: 10: 1 was developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to the spot colour developing clear; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(3) content of paeoniflorin is measured:
The preparation of reference substance solution: it is an amount of to get the Paeoniflorin reference substance, and accurate the title decides, and puts in the volumetric flask, adds Diluted Alcohol and makes the solution that every 1ml contains 0.1mg, promptly;
The preparation of need testing solution: it is an amount of to get this product water-honeyed pill, and porphyrize is got about 2g, and accurate the title decides; Or get big honeyed pills under the weight differential item, shred, mixing is got about 3g, accurate claim fixed.Put in the tool plug conical flask, the accurate Diluted Alcohol 15ml that adds claims decide weight, and sonicated 30 minutes is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with Diluted Alcohol, shakes up, and filtration is got subsequent filtrate, promptly;
Use high effective liquid chromatography for measuring: be filling agent with the octadecylsilane chemically bonded silica; With 15: 85 acetonitriles-0.1% phosphoric acid solution is moving phase; The detection wavelength is 232nm; Number of theoretical plate calculates by the Paeoniflorin peak should be not less than 3000.Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject liquid chromatograph, measure; Content of paeoniflorin in the calculation sample.
The present invention draws by test, and this product contains the radix paeoniae rubrathe with Paeoniflorin (C 23H 28O 11) meter, the every 1g of water-honeyed pill must not be less than 0.2mg; The every ball of big honeyed pills must not be less than 1.0mg.
The meaning that quality standard of the present invention improves is: the invention provides the qualitative identification to scutelloside, burdock glycosides, made best test sample preparation method, found suitable developping agent, can carry out effective qualitative identification to said preparation.The invention provides the content of paeoniflorin assay method in addition, adopt high performance liquid chromatography that Paeoniflorin is carried out assay, made best test sample preparation method and moving phase compound method, improved the content of paeoniflorin accuracy in detection greatly.The foundation of this method helps on the market true and false quality to this Chinese traditional compound medicine and differentiates.
Four, embodiment:
Embodiment 1:
With honeysuckle, the capsule of weeping forsythia, radix scrophulariae, Radix Isatidis, the radix paeoniae rubrathe, the root of large-flowered skullcap, mulberry leaf, chrysanthemum, the root of purple-flowered peucedanum, semen armeniacae amarae (fire is single), great burdock achene, rhizoma alismatis, the sterculia seed, stiff silkworm (bran stir-fry), cicada slough, Oroxylum indicum ten Six-element medicines, be ground into fine powder, sieve mixing; Every 100g powder adds refined honey 35~50g and an amount of water, pill, and drying is used the activated charcoal dressing, makes water-honeyed pill, and its detection method may further comprise the steps:
(1) gets this product water-honeyed pill 5g, grind; Add zeyssatite 4g, grind well; Add methyl alcohol 40ml, sonicated 30 minutes filters, and filtrate evaporate to dryness, residue add water 20ml makes dissolving, transfers pH value to being about 2 with watery hydrochloric acid, extracts 2 times with the ethyl acetate jolting, and each 20ml merges extract, evaporate to dryness; Residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets the scutelloside reference substance, adds methyl alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin-layered chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with 5: 3: 1: ethyl acetate-butanone of 1-formic acid-aqueous solution was a developping agent, launch, take out, dry, spray is with 2% ferric trichloride ethanolic solution; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(2) get this product water-honeyed pill 5g, grind; Add zeyssatite 4g, grind well; The mixed solution 40ml that adds ethyl acetate-methyl alcohol of 2: 1, sonicated 20 minutes filters, and filtrate evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution; Other gets burdock glycosides reference substance, adds methyl alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin-layered chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with methenyl choloride-methanol-waters of 40: 10: 1 was developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to the spot colour developing clear; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(3) content of paeoniflorin is measured:
The preparation of reference substance solution: it is an amount of to get the Paeoniflorin reference substance, and accurate the title decides, and puts in the volumetric flask, adds Diluted Alcohol and makes the solution that every 1ml contains 0.1mg, promptly;
The preparation of need testing solution: it is an amount of to get this product water-honeyed pill, and porphyrize is got about 2g, and accurate the title decides; Put in the tool plug conical flask, the accurate Diluted Alcohol 15ml that adds claims decide weight, and sonicated 30 minutes is put coldly, weighs again, supplies the weight that subtracts mistake with Diluted Alcohol, shakes up, and filtration is got subsequent filtrate, promptly;
Use high effective liquid chromatography for measuring: be filling agent with the octadecylsilane chemically bonded silica; With 15: 85 acetonitriles-0.1% phosphoric acid solution is moving phase; The detection wavelength is 232nm; Number of theoretical plate calculates by the Paeoniflorin peak should be not less than 3000.Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject liquid chromatograph, measure; Content of paeoniflorin in the calculation sample.
Repeat above-mentioned steps once, the mean value of paeoniflorin content is 0.35mg/g in the calculation sample.
Embodiment 2:
With honeysuckle, the capsule of weeping forsythia, radix scrophulariae, Radix Isatidis, the radix paeoniae rubrathe, the root of large-flowered skullcap, mulberry leaf, chrysanthemum, the root of purple-flowered peucedanum, semen armeniacae amarae (fire is single), great burdock achene, rhizoma alismatis, the sterculia seed, stiff silkworm (bran stir-fry), cicada slough, Oroxylum indicum ten Six-element medicines, be ground into fine powder, sieve mixing; Every 100g powder or add refined honey 110g~130g and make big honeyed pills, its detection method may further comprise the steps:
(1) gets big honeyed pills 8g, shred, add zeyssatite 4g, grind well; Add methyl alcohol 40ml, sonicated 30 minutes filters, and filtrate evaporate to dryness, residue add water 20ml makes dissolving, transfers pH value to being about 2 with watery hydrochloric acid, extracts 2 times with the ethyl acetate jolting, and each 20ml merges extract, evaporate to dryness; Residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets the scutelloside reference substance, adds methyl alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin-layered chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with 5: 3: 1: ethyl acetate-butanone of 1-formic acid-aqueous solution was a developping agent, launch, take out, dry, spray is with 2% ferric trichloride ethanolic solution; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(2) get big honeyed pills 8g, shred, add zeyssatite 4g, grind well; The mixed solution 40ml that adds ethyl acetate-methyl alcohol of 2: 1, sonicated 20 minutes filters, and filtrate evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution; Other gets burdock glycosides reference substance, adds methyl alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin-layered chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with methenyl choloride-methanol-waters of 40: 10: 1 was developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to the spot colour developing clear; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(3) content of paeoniflorin is measured:
The preparation of reference substance solution: it is an amount of to get the Paeoniflorin reference substance, and accurate the title decides, and puts in the volumetric flask, adds Diluted Alcohol and makes the solution that every 1ml contains 0.1mg, promptly;
The preparation of need testing solution: get the big honeyed pills under the weight differential item, shred, mixing is got about 3g, and accurate the title decides.Put in the tool plug conical flask, the accurate Diluted Alcohol 15ml that adds claims decide weight, and sonicated 30 minutes is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with Diluted Alcohol, shakes up, and filtration is got subsequent filtrate, promptly;
Use high effective liquid chromatography for measuring: be filling agent with the octadecylsilane chemically bonded silica; With 15: 85 acetonitriles-0.1% phosphoric acid solution is moving phase; The detection wavelength is 232nm; Number of theoretical plate calculates by the Paeoniflorin peak should be not less than 3000.Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject liquid chromatograph, measure; Content of paeoniflorin in the calculation sample.
Repeat above-mentioned steps once, the mean value of paeoniflorin content is the 1.54mg/ ball in the calculation sample.
With embodiment 1 and embodiment 2 described quality determining method repetition tests 8 times, draw the mean value of paeoniflorin content (mg/ ball) in the mean value of paeoniflorin content in the water-honeyed pill (mg/g) and the big honeyed pills, the results are shown in following table:
Figure C20071001762100091
Laboratory report:
1, instrument and reagent
Instrument: TSP2000 high performance liquid chromatograph, P2000 binary gradient pump, UV1000 UV-detector, N2000 chromatographic work station.
Reagent: the second eyeball is a chromatorgaphy reagent, and water is redistilled water, and it is pure that other reagent is analysis.
Reference substance: Paeoniflorin, lot number are 0736-200117, for assay usefulness, are provided by Nat'l Pharmaceutical ﹠ Biological Products Control Institute.
Test sample: Kaiyinwan ball, lot number: 030539; Specification: per 10 heavy 1g; Packing: plastic bottle, every bottled 36g is produced by our company.
2, chromatographic condition
Chromatographic column: 5 μ m, 250mm * 4.6mm Poaris-ODS post
Moving phase: 15: 85 second eyeball-0.1% phosphoric acid solution
Flow velocity: 1.0ml/min;
Column temperature: 25 ℃;
Detect wavelength: 232nm;
The selection of 3, pre-treatment condition
The investigation of extracting method: precision takes by weighing the about 2g of this product water-honeyed pill, put in the tool plug conical flask, the accurate Diluted Alcohol 15ml that adds claims to decide weight, extracted 30 minutes with different extracting method respectively, extract put cold after, supply the weight that subtracts mistake with Diluted Alcohol, shake up, filter, get subsequent filtrate, sample introduction records its content.The results are shown in Table 1
The comparison of table 1 Different Extraction Method
Figure C20071001762100101
Above result shows: sonicated is higher slightly than the content of refluxing extraction, and refluxing extraction impurity is more, so determine with the ultrasonic Extraction to be extracting method.
The investigation of extraction time: precision takes by weighing the about 2g of this product water-honeyed pill, puts in the tool plug conical flask, and the accurate Diluted Alcohol 15ml that adds claims to decide weight, sonicated different time is respectively put coldly, supplies the weight that subtracts mistake with Diluted Alcohol, shakes up, filter, get subsequent filtrate, sample introduction records its content.The results are shown in Table 2
The investigation of table 2 different extraction times
Figure C20071001762100102
Above result shows: ultrasonic 20 minutes, content was constant substantially, but considered and extract fully, so definite 30 minutes is the ultrasonic Extraction time.
4, methodological study
The investigation of the range of linearity: precision is measured Paeoniflorin reference substance solution (0.2048mg/ml) 1,2,4,6,8,10 μ l sample introductions, and the record chromatogram is measured its peak area (the results are shown in Table 3); And with peak area value (A) sample size (B) is returned, typical curve equation method.
Table 3 Paeoniflorin reference substance measurement result
Figure C20071001762100103
A=49161.62466 B=1415901.942 r=0.9993
And with peak area value (A) to sample size (B) mapping, a straight line.
Above result shows: in 0.2048-2.048 μ g scope, Paeoniflorin peak area value and sample size have good linear relationship.
The precision test: the accurate Paeoniflorin reference substance solution 10 μ l that draw, repeat sample introduction 5 times, measure.The results are shown in Table 4
The test of table 4 Paeoniflorin precision
Figure C20071001762100111
The result shows: precision is good.
The preparation of blank solution and mensuration: in prescription ratio and technology, preparation does not contain the blank sample of the radix paeoniae rubrathe, prepares negative control solution by the preparation method of need testing solution, measures.In the blank chromatogram, there be not the peak appearance mutually nearby with reference substance peak retention time.
Stability test: sample thief (lot number: 030539) and reference substance solution respectively at 0,0.5,1,2,4 hours sample introduction 10 μ l measure.The results are shown in Table 5
Table 5 stability test result
Test findings shows that reference substance and sample solution are all good at 4 hours internal stabilities.
Replica test: by the content assaying method of drafting, to same batch sample (lot number: 030539) prepare the sample test liquid respectively, record peak area and calculate content.The results are shown in Table 6
The test of table 6 sample reappearance
Figure C20071001762100113
The result shows: by the content assaying method of drafting, reappearance is good.
Average recovery test: precision takes by weighing the sample of known content, and (lot number: 030539) an amount of, it is an amount of to add reference substance solution respectively, prepares sample by above-mentioned sample preparation methods and chromatographic condition, sample introduction.With following formula calculate recovery rate.The results are shown in Table 7
Figure C20071001762100121
Table 7 sample recovery rate test findings
Figure C20071001762100122
Test findings shows: all between 95~105%, application of sample reclaims good the recovery.
5, sample size is measured: accurate respectively reference substance solution and the sample solution drawn, press method under the text assay item, and measure.(the results are shown in Table 8)
Paeoniflorin content measurement result (n=2) in table 8 sample
Figure C20071001762100123
According to above-mentioned test findings, consider crude drug source, and preparation production, factors such as storage so the tentative every gram of this product contains the radix paeoniae rubrathe in the Paeoniflorin amount, must not be less than 0.20mg.
6, the assay of radix paeoniae rubrathe medicinal material: get the about 0.1g of this product powder, accurate claim surely, put in the tool plug conical flask, precision adds Diluted Alcohol 15ml, claims decide weight, and sonicated 30 minutes is put coldly, supplies the weight that subtracts mistake with Diluted Alcohol, shakes up, and filtration is got subsequent filtrate promptly.The results are shown in Table 9.
Paeoniflorin content measurement result (n=2) in the radix paeoniae rubrathe medicinal material of the different place of production of table 9
Figure C20071001762100131
According to measurement result, consider factor such as the medicinal material place of production, processing processs of preparing Chinese medicine, storage and " content limit regulation in the Chinese pharmacopoeia is fixed tentatively the content total amount and is not less than 1.8%.

Claims (2)

1, a kind of quality determining method of Chinese medicine preparation Kaiyinwan ball is with honeysuckle, the capsule of weeping forsythia, radix scrophulariae, Radix Isatidis, the radix paeoniae rubrathe, the root of large-flowered skullcap, mulberry leaf, chrysanthemum, the root of purple-flowered peucedanum, amygdalate
Figure C2007100176210002C1
, great burdock achene, rhizoma alismatis, the sterculia seed, bran stiff silkworm, cicada slough, the Oroxylum indicum ten Six-element medicines fried, be ground into fine powder, sieve mixing; Every 100g powder adds refined honey 35~50g and an amount of water, pill, and drying is used the activated charcoal dressing, makes water-honeyed pill; Or add refined honey 110g~130g and make big honeyed pills, that is, it is characterized in that may further comprise the steps:
(1) gets this product water-honeyed pill 5g, grind; Or get big honeyed pills 8g, and shred, add zeyssatite 4g, grind well; Add methyl alcohol 40ml, sonicated 30 minutes filters, and filtrate evaporate to dryness, residue add water 20ml makes dissolving, transfers pH value to 2 with watery hydrochloric acid, extracts 2 times with the ethyl acetate jolting, and each 20ml merges extract, evaporate to dryness; Residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets the scutelloside reference substance, adds methyl alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin-layered chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with 5: 3: 1: ethyl acetate-butanone of 1-formic acid-aqueous solution was a developping agent, launch, take out, dry, spray is with 2% ferric trichloride ethanolic solution; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(2) get this product water-honeyed pill 5g, grind; Or get big honeyed pills 8g, and shred, add zeyssatite 4g, grind well; The mixed solution 40ml that adds ethyl acetate-methyl alcohol of 2: 1, sonicated 20 minutes filters, and filtrate evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution; Other gets burdock glycosides reference substance, adds methyl alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin-layered chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with methenyl choloride-methanol-waters of 40: 10: 1 was developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to the spot colour developing clear; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(3) content of paeoniflorin is measured:
The preparation of reference substance solution: it is an amount of to get the Paeoniflorin reference substance, and accurate the title decides, and puts in the volumetric flask, adds Diluted Alcohol and makes the solution that every 1ml contains 0.1mg, promptly;
The preparation of need testing solution: it is an amount of to get this product water-honeyed pill, and porphyrize is got 2g, and accurate the title decides; Or get big honeyed pills under the weight differential item, shred, mixing is got 3g, accurate claim fixed; Put in the tool plug conical flask, the accurate Diluted Alcohol 15ml that adds claims decide weight, and sonicated 30 minutes is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with Diluted Alcohol, shakes up, and filtration is got subsequent filtrate, promptly;
Use high effective liquid chromatography for measuring: be filling agent with the octadecylsilane chemically bonded silica; With 15: 85 acetonitriles-0.1% phosphoric acid solution is moving phase; The detection wavelength is 232nm; Number of theoretical plate calculates by the Paeoniflorin peak should be not less than 3000; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject liquid chromatograph, measure; Content of paeoniflorin in the calculation sample.
2, the quality determining method of a kind of Chinese medicine preparation Kaiyinwan ball as claimed in claim 1, it is characterized in that: described Chinese medicine preparation contains the radix paeoniae rubrathe in Paeoniflorin, and the every 1g of water-honeyed pill must not be less than 0.2mg; The every ball of big honeyed pills must not be less than 1.0mg.
CNB2007100176210A 2007-04-04 2007-04-04 Method for inspecting Chinese-medicinal preparation Kaiyinwan Active CN100432670C (en)

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金嗓颗粒的制备及薄层色谱鉴别. 陈雅等.制剂技术,第15卷第1期. 2006 *

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