CN101029890A - Method for inspecting Chinese-medicinal preparation Kaiyinwan - Google Patents
Method for inspecting Chinese-medicinal preparation Kaiyinwan Download PDFInfo
- Publication number
- CN101029890A CN101029890A CN 200710017621 CN200710017621A CN101029890A CN 101029890 A CN101029890 A CN 101029890A CN 200710017621 CN200710017621 CN 200710017621 CN 200710017621 A CN200710017621 A CN 200710017621A CN 101029890 A CN101029890 A CN 101029890A
- Authority
- CN
- China
- Prior art keywords
- solution
- reference substance
- paeoniflorin
- adds
- methyl alcohol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Cosmetics (AREA)
- Medicines Containing Plant Substances (AREA)
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
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 (Dan), 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 (Dan), 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 (Dan), 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:
| Sequence number | Step 1 | Step 2 | Paeoniflorin content in the water-honeyed pill (mg/g) | Paeoniflorin content in the big honeyed pills (mg/ ball) | ||||
| For the first time | For the second time | Mean value | For the first time | For the second time | Mean value | |||
| 1 | Detect | Detect | 0.39 | 0.35 | 0.37 | 1.78 | 1.72 | 1.75 |
| 2 | Detect | Detect | 0.32 | 0.34 | 0.33 | 1.25 | 1.18 | 1.21 |
| 3 | Detect | Detect | 0.42 | 0.44 | 0.43 | 1.61 | 1.64 | 1.62 |
| 4 | Detect | Detect | 0.47 | 0.41 | 0.44 | 1.97 | 1.93 | 1.95 |
| 5 | Detect | Detect | 0.46 | 0.42 | 0.44 | 1.35 | 1.31 | 1.33 |
| 6 | Detect | Detect | 0.35 | 0.39 | 0.37 | 1.49 | 1.45 | 1.47 |
| 7 | Detect | Detect | 0.37 | 0.32 | 0.35 | 1.39 | 1.42 | 1.41 |
| 8 | Detect | Detect | 0.31 | 0.28 | 0.30 | 1.52 | 1.57 | 1.54 |
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
| Extracting method | Ultrasonic | Reflux |
| Content of paeoniflorin (mg/g) | 0.7736 | 0.7247 |
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
| Ultrasonic time (min) | 10 | 20 | 30 | 45 |
| Content of paeoniflorin (mg/g) | 0.7156 | 0.7731 | 0.7736 | 0.7660 |
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
| Sample size (g) | 0.2048 | 0.4096 | 0.8192 | 1.2288 | 1.6384 | 2.048 |
| Peak area value | 289537 | 636440 | 1211230 | 1775732 | 2352561 | 2961144 |
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
| Test number (TN) | 1 | 2 | 3 | 4 | 5 | RSD(％) |
| The Paeoniflorin peak area value | 1468433 | 1467564 | 1466836 | 1465304 | 1462439 | 0.16 |
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
| Minute | 0 | 0.5 | 1 | 2 | 4 | RSD(％) |
| Sample | 1502565 | 1514154 | 1506056 | 1512772 | 1509548 | 0.32 |
| The Paeoniflorin reference substance | 1476456 | 1478090 | 1472514 | 1470629 | 1479565 | 0.26 |
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
| Tested number | 1 | 2 | 3 | 4 | 5 | RSD(％) |
| Paeoniflorin (mg/g) | 0.7736 | 0.7736 | 0.7707 | 0.7736 | 0.7721 | 0.17 |
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
Table 7 sample recovery rate test findings
| Numbering | Sample heavy (g) | Paeoniflorin content (mg) | Add Paeoniflorin amount (mg) | The amount that records (mg) | The recovery (%) | Average recovery rate (%) | RSD (％) |
| 1 2 3 4 5 6 | 0.6888 0.6779 1.2145 1.2648 1.7114 1.8307 | 0.533 0.524 0.939 0.978 1.324 1.416 | 1.024 1.024 1.024 1.024 1.024 1.024 | 1.536 1.512 1.919 2.015 2.322 2.447 | 97.9 96.5 95.7 101.3 97.5 100.7 | 98.3 | 2.3 |
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
| Lot number | The containing of Paeoniflorin (mg/g) | Paeoniflorin average content (mg/g) |
| 010534 010955 011072 011282 020514 020839 030309 030539 | 0.221 0.239 0.381 0.399 0.308 0.332 0.419 0.421 0.464 0.476 0.454 0.466 0.345 0.355 0.361 0.379 | 0.23 0.39 0.32 0.42 0.47 0.46 0.35 0.37 |
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
| The place of production | The Inner Mongol | Shanxi | Yunnan |
| Content (%) | 2.25 | 3.98 | 1.84 |
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, semen armeniacae amarae
Great burdock achene, rhizoma alismatis, the sterculia seed, stiff silkworm (bran stir-fry), cicada slough, Oroxylum indicum ten Six-element medicines are 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 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.
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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100176210A CN100432670C (en) | 2007-04-04 | 2007-04-04 | Method for inspecting Chinese-medicinal preparation Kaiyinwan |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100176210A CN100432670C (en) | 2007-04-04 | 2007-04-04 | Method for inspecting Chinese-medicinal preparation Kaiyinwan |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101029890A true CN101029890A (en) | 2007-09-05 |
| CN100432670C CN100432670C (en) | 2008-11-12 |
Family
ID=38715353
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007100176210A Active CN100432670C (en) | 2007-04-04 | 2007-04-04 | Method for inspecting Chinese-medicinal preparation Kaiyinwan |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100432670C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102297926A (en) * | 2011-07-12 | 2011-12-28 | 刘金伶 | Rapid TLC identification and three-component simultaneous quantitative determination method for antitussive tablets |
| CN101564514B (en) * | 2009-06-12 | 2013-06-05 | 杨文龙 | Method for analyzing children Fengreqing particle |
| CN115420816A (en) * | 2022-07-21 | 2022-12-02 | 广东万年青制药股份有限公司 | Content determination method of traditional Chinese medicine composition for nourishing yin and cooling blood |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0959170A (en) * | 1995-08-11 | 1997-03-04 | Tsumura & Co | Separation and purification of baicalin and baicalein |
| WO2002032438A1 (en) * | 2000-09-13 | 2002-04-25 | Jiangsu Kanion Pharmaceutical Co. | Pharmaceutical composition treating gynecological blood stasis diseases, cardio and cerebral vascular diseases, respiratory diseases and the like |
| CN1368130A (en) * | 2001-02-02 | 2002-09-11 | 杨孟君 | Nano medicine 'Jinsang Liyan' and its preparing process |
-
2007
- 2007-04-04 CN CNB2007100176210A patent/CN100432670C/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101564514B (en) * | 2009-06-12 | 2013-06-05 | 杨文龙 | Method for analyzing children Fengreqing particle |
| CN102297926A (en) * | 2011-07-12 | 2011-12-28 | 刘金伶 | Rapid TLC identification and three-component simultaneous quantitative determination method for antitussive tablets |
| CN115420816A (en) * | 2022-07-21 | 2022-12-02 | 广东万年青制药股份有限公司 | Content determination method of traditional Chinese medicine composition for nourishing yin and cooling blood |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100432670C (en) | 2008-11-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101766771A (en) | Quality control method of medicine for gynecopathy treatment | |
| CN106370738B (en) | Fingerprint quality determination method for periplaneta americana medicinal material | |
| CN101028460B (en) | Method for inspecting throat-clearing Chinese medicinal pills | |
| CN1857589A (en) | Method of measuring icariin and epimedin c content in Xianlinggubao preparation | |
| CN1785255A (en) | Method for quality control of traditional Chinese medicine prepns. | |
| CN101028388B (en) | Quality inspection of Chinese-medicinal preparation for treating shortsighness and asthenopia | |
| CN101444589A (en) | Quality standard of Fenqing Wulin Wan and inspection method thereof | |
| CN102579734B (en) | Traditional Chinese medicine composition of bone healing medicine, preparing method thereof and detecting method thereof | |
| CN101029889A (en) | Method for inspecting Chinese medicinal preparation quality in treatment of old man eyes dieases | |
| CN102068649B (en) | Quality control method for gastric condition-regulating pill as traditional Chinese preparation | |
| CN101029890A (en) | Method for inspecting Chinese-medicinal preparation Kaiyinwan | |
| CN101028487A (en) | Chinese-medicinal preparation for treating eyeground bleeding and method for inspecting vision-improving prescription quality | |
| CN102552515A (en) | Quality detection method for blood-nourishing Chinese angelica syrup | |
| CN100369614C (en) | Quality control method of compound gallblader freeflow solid preparation | |
| CN102068656A (en) | Quality control method for traditional Chinese medicinal preparation epilepsy pills | |
| CN103316102A (en) | Detection method for external traditional Chinese medicine preparation for treating haemorrhoids | |
| CN101352565A (en) | Quality control method of granular formulation for activating blood and resolving stasis, detoxifying and dispersing swelling | |
| CN102707006A (en) | Quality detection method of cudrania tricuspidata formula granules | |
| CN100370253C (en) | Method for quality control of Qianbai biyan solid prepn. for treating rhinitis | |
| CN101700306A (en) | Quality control method of Rupixiao preparation | |
| CN101028474B (en) | Method for inspecting the quality of Chinese preparation with Yang-and kidney tonifying functions | |
| CN101380441A (en) | A quality standard of Chinese medicine preparation for regulating menstruation, nourishing blood, warming uterus, dispelling cold and relieving pain and its inspection method | |
| CN102068566B (en) | Detection method for Yinchen Wudan pills for treating damp-heat jaundice | |
| CN102068599B (en) | Detection method for phlegm eliminating and asthma relieving cough syrup | |
| CN1883604B (en) | Detection method of compound preparation of red sage root and cape jasmine for treating acute and chronic hepatitis |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |