CN101306139A - Quality control method of Biyan Qingdu granule - Google Patents
Quality control method of Biyan Qingdu granule Download PDFInfo
- Publication number
- CN101306139A CN101306139A CNA200810029030XA CN200810029030A CN101306139A CN 101306139 A CN101306139 A CN 101306139A CN A200810029030X A CNA200810029030X A CN A200810029030XA CN 200810029030 A CN200810029030 A CN 200810029030A CN 101306139 A CN101306139 A CN 101306139A
- Authority
- CN
- China
- Prior art keywords
- solution
- keli
- methanol
- layer chromatography
- add
- 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.)
- Pending
Links
Landscapes
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention relates to a method used for controlling the quality of nose larynx toxin-clearing granules, which comprises the steps of (1) discriminating flos chrysanthemi indici contained in the nose larynx toxin-clearing granules by adopting the thin-layer chromatography, and comparing the nose larynx toxin-clearing granules with linarin; (2) discriminating radix zanthoxyli contained in the nose larynx toxin-clearing granules by adopting the thin-layer chromatography; (3) detecting the content of gentiopicrin in the nose larynx toxin-clearing granules by adopting the high efficiency liquid chromatography. The control method overcomes the defects of the prior chemical discrimination method, namely low specialty of the prior chemical discrimination method, low specialty of self-heal in the prior thin-layer chromatography, no effective ingredients for comparison in the prior thin-layer chromatography for discriminating flos chrysanthemi indici, and seriously tailing, and no methods for detecting the content of effective ingredients. The specialty and the quality stability of the method provided by the invention are improved; and the safety and the effectiveness of the granules are ensured.
Description
Technical field
The present invention relates to the method for quality control of Chinese patent medicine, specifically, the present invention relates to a kind of method of quality control of BIYAN QINGDU KELI.
Background technology
BIYAN QINGDU KELI is the Chinese patent medicine (compound Chinese medicinal preparation) of a kind of heat-clearing and toxic substances removing, dissipating phlegm and resolving masses, has used for many years in China, and the clinical pyretic toxicity that is used for pents up nasopharynx, nasopharyngeal sore pain, and the nasopharynx part chronic inflammatory disease, disease such as secretions increase behind the nasopharyngeal carcinoma radiotherapy, curative effect is sure.BIYAN QINGDU KELI is prepared from according to the particulate common process of Chinese patent medicine by Chinese medicine Flos Chrysanthemi Indici, Fructus Xanthii, Rhizoma Paridis, radix rubi parvifol, Radix Zanthoxyli, Spica Prunellae, Radix Gentianae, Radix Codonopsis.This standard is recorded the national drug standards in National Drug Administration.The authentication method of this standard includes (1) and detects flavones ingredient by the method that magnesium powder, hydrochloric acid take on a red color Flavonoid substances, and Flos Chrysanthemi Indici, Spica Prunellae contain flavones ingredient in the BIYAN QINGDU KELI; (2) make the lactone material show red method by the diazonium p-nitrobenzoic acid and detect yejuhua lactone, Flos Chrysanthemi Indici contains yejuhua lactone in the BIYAN QINGDU KELI; (3) by containing Flos Chrysanthemi Indici, Spica Prunellae, gentiopicrin in the thin layer chromatography detection BIYAN QINGDU KELI, but the above two the obvious specificity of chemical differential method is not strong, the thin layer chromatography specificity of Spica Prunellae is not strong yet, Flos Chrysanthemi Indici adopts isobutyltrimethylmethane .-benzene-chloroform-acetic acid ethyl ester-formic acid (12: 6: 3: 6: 1) serious for the developing solvent hangover, therefore this method is difficult to effectively differentiate BIYAN QINGDU KELI, more, can not effectively control the quality of its product owing to no active constituent content measuring method.
Summary of the invention
Purpose of the present invention is exactly the shortcoming for the quality standard that overcomes present BIYAN QINGDU KELI, provides that a kind of specificity is strong, the method for quality control of BIYAN QINGDU KELI that can more accurate control product quality.
The present invention realizes like this.
The present invention adopts: (1) thin layer chromatography differentiates that BIYAN QINGDU KELI contains Flos Chrysanthemi Indici, and in addition with linarin in contrast; (2) thin layer chromatography is differentiated in the BIYAN QINGDU KELI and is contained Radix Zanthoxyli; (3) the employing high performance liquid chromatography detects the gentiopicroside in different morphological in the BIYAN QINGDU KELI.
In fact, linarin is one of active ingredient of Flos Chrysanthemi Indici, and Radix Gentianae is one of BIYAN QINGDU KELI principal agent, and gentiopicrin is one of active ingredient of Radix Gentianae, by the content of the Radix Gentianae in the Determination of gentiopicroside reflection preparation.
Thin layer chromatography differentiates that the preferable condition that contains Flos Chrysanthemi Indici in the BIYAN QINGDU KELI is:
Get this product, add hot water and make dissolving, put coldly, use water saturated n-butanol extraction, merge n-butyl alcohol liquid, evaporate to dryness, residue add methanol makes dissolving, filters, and filtrate is as need testing solution.Other gets the Flos Chrysanthemi Indici control medicinal material, adds water and is heated to boiling, puts coldly, uses water saturated n-butanol extraction, merges n-butyl alcohol liquid, and evaporate to dryness, residue add methanol makes dissolving, filters, and filtrate is made control medicinal material solution.Get the linarin reference substance again, add methanol and make the solution that every 1ml contains about 0.2mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw above-mentioned three kinds of solution, put respectively on same polyamide film, (2: 5: 5: 1) be developing solvent, expansion was taken out with normal hexane-ethyl acetate-butanone-formic acid, dry, spray is with 2% aluminum trichloride solution, and hot blast drying is put under the ultra-violet lamp (365nm) and inspected.In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color respectively.
Thin layer chromatography differentiates that the preferable condition that contains Radix Zanthoxyli in the BIYAN QINGDU KELI is:
Get this product, add hydrochloric acid solution (1 → 50, the concentrated hydrochloric acid that is about to 1 volume is diluted with water to 50 volumes) heating in water bath makes dissolving, add 20% sodium hydroxide solution adjust pH to 11～12 again, put in the separatory funnel, add the ethyl acetate jolting and extract, standing demix, merge upper strata liquid, evaporate to dryness, residue add methanol makes dissolving as need testing solution.Other gets the Radix Zanthoxyli control medicinal material, add hydrochloric acid solution (1 → 50) heating in water bath 20 minutes, put coldly, filter, add 20% sodium hydroxide solution adjust pH to 11～12 again, put in the separatory funnel, add the ethyl acetate jolting and extract, standing demix merges upper strata liquid, evaporate to dryness, residue add methanol makes dissolving make control medicinal material solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw above-mentioned need testing solution, control medicinal material solution, put respectively on same silica gel g thin-layer plate, it is in the expansion cylinder of developing solvent that lamellae is put with normal hexane-ethyl acetate-methanol-isopropyl alcohol-strong ammonia solution (20: 5: 1: 1: 0.12), presaturation 20 minutes launches, and takes out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
The preferable condition of the gentiopicrin in the high effective liquid chromatography for measuring BIYAN QINGDU KELI is:
[assay] measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (23: 77) is a mobile phase; Detect wavelength: 270nm.Number of theoretical plate calculates by the gentiopicrin peak should be not less than 3000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the gentiopicrin reference substance, adds 30% methanol and make the solution that every 1ml contains 40 μ g, promptly.
This product is got in the preparation of need testing solution, and porphyrize is got about 1g, accurate claims surely, puts in the 25ml volumetric flask, adds 30% methanol to nearly scale, and supersound process 10 minutes is put coldly, adds 30% methanol to scale, shakes up, and gets supernatant, promptly.
Accurate respectively reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly.
The every 1g of this product contains Radix Gentianae with gentiopicrin (C
16H
20O
9) meter, must not be less than 0.5mg.
This assay method is through methodology checking, has that separating degree is good, highly sensitive, the accuracy advantages of higher.Regression equation is y=23239954.6745x+17336.0833 (correlation coefficient r=0.9999), shows that gentiopicrin has good linear relationship in 0.00864～0.1728mg/ml concentration range; The accuracy test average recovery rate is 98.0%, RSD%=0.63%; Repeated experiment RSD%=0.40%.
10 batches of test sample measurement results
The method of quality control of BIYAN QINGDU KELI of the present invention, there is no active ingredient contrast in not strong, the former Flos Chrysanthemi Indici thin layer chromatography of specificity that has overcome not strong, the former thin layer chromatography Spica Prunellae of existing chemical discrimination method specificity and the shortcoming serious and that do not have active constituent content measuring method of trailing, improve the specificity and the quality stability of BIYAN QINGDU KELI method of quality control, guaranteed the safety and the effectiveness of people's medications.
The specific embodiment
The invention will be further described below in conjunction with embodiment.
The lot number of getting applicant's production is 5072 BIYAN QINGDU KELI.
[discriminating]
(1) get this product 5g, add hot water 10ml and make dissolving, put coldly, with water saturated n-butanol extraction 2 times, each 20ml merges n-butyl alcohol liquid, and evaporate to dryness, residue add methanol 5ml makes dissolving, filters, and filtrate is as need testing solution.Other gets Flos Chrysanthemi Indici control medicinal material 0.5g, adds water 20ml, is heated to boiling 15 minutes, from " put cold, with water saturated n-butanol extraction 2 times ", makes control medicinal material solution with the need testing solution preparation method.Get the linarin reference substance again, add methanol and make the solution that every 1ml contains 0.2mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 2 μ l of above-mentioned three kinds of solution, put respectively on same polyamide film, (2: 5: 5: 1) be developing solvent, expansion was taken out with normal hexane-ethyl acetate-butanone-formic acid, dry, spray is with 2% aluminum trichloride solution, and hot blast drying is put under the ultra-violet lamp (365nm) and inspected.In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color respectively.
(2) get this product 20g, add hydrochloric acid solution (1 → 50) 50ml heating in water bath and make dissolving, add 20% sodium hydroxide solution adjust pH to 11～12 again, put in the separatory funnel, add the ethyl acetate jolting and extract 2 times, each 30ml, standing demix, merge upper strata liquid, evaporate to dryness, residue add methanol 0.5ml makes dissolving as need testing solution.Other gets Radix Zanthoxyli control medicinal material 0.25g, adds hydrochloric acid solution (1 → 50) 50ml heating in water bath 20 minutes, puts coldly, filters, and from " adding 20% sodium hydroxide solution adjust pH to 11～12 again ", makes control medicinal material solution with the need testing solution preparation method.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw above-mentioned need testing solution 6 μ l, control medicinal material solution 1 μ l, put respectively on same silica gel g thin-layer plate, it is in the expansion cylinder of developing solvent that lamellae is put with normal hexane-ethyl acetate-methanol-isopropyl alcohol-strong ammonia solution (20: 5: 1: 1: 0.12), presaturation 20 minutes launches, and takes out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
[inspection] should meet every regulation relevant under the granule item (an appendix I of Chinese Pharmacopoeia version in 2005 C).
[assay] measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (23: 77) is a mobile phase; Detect wavelength: 270nm.Number of theoretical plate calculates by the gentiopicrin peak should be not less than 3000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the gentiopicrin reference substance, adds 30% methanol and make the solution that every 1ml contains 40 μ g, promptly.
This product 20g is got in the preparation of need testing solution, and porphyrize is got about 1g, accurate claims surely, puts in the 25ml volumetric flask, adds 30% methanol to nearly scale, and supersound process 10 minutes is put coldly, adds 30% methanol to scale, shakes up, and gets supernatant, promptly.
Accurate respectively reference substance solution and each the 20 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
The every 1g of this product contains Radix Gentianae with gentiopicrin (C
16H
20O
9) meter, must not be less than 0.5mg.
It is 1.0738mg that the every 1g of this lot number product contains gentiopicrin.
Claims (4)
1, a kind of method of quality control of BIYAN QINGDU KELI comprises that employing (1) thin layer chromatography discriminating BIYAN QINGDU KELI contains Flos Chrysanthemi Indici, and in addition with linarin in contrast; (2) thin layer chromatography is differentiated in the BIYAN QINGDU KELI and is contained Radix Zanthoxyli; (3) the employing high performance liquid chromatography detects the gentiopicroside in different morphological in the BIYAN QINGDU KELI.
2, the method for quality control of a kind of BIYAN QINGDU KELI according to claim 1, it is characterized in that the condition that contains Flos Chrysanthemi Indici in the thin layer chromatography discriminating BIYAN QINGDU KELI is: get this product, add hot water and make dissolving, put coldly, use water saturated n-butanol extraction, merge n-butyl alcohol liquid, evaporate to dryness, residue adds methanol makes dissolving, filters, and filtrate is as need testing solution; Other gets the Flos Chrysanthemi Indici control medicinal material, adds water and is heated to boiling, puts coldly, uses water saturated n-butanol extraction, merges n-butyl alcohol liquid, and evaporate to dryness, residue add methanol makes dissolving, filters, and filtrate is made control medicinal material solution; Get the linarin reference substance again, add methanol and make the solution that every 1ml contains about 0.2mg, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned three kinds of solution, put respectively on same polyamide film, be developing solvent with normal hexane-ethyl acetate-butanone-formic acid, launch, take out, to dry, spray is with 2% aluminum trichloride solution, and hot blast drying is put under the ultra-violet lamp and is inspected; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color respectively.
3, the method for quality control of a kind of BIYAN QINGDU KELI according to claim 1, it is characterized in that the preferable condition that contains Radix Zanthoxyli in the thin layer chromatography discriminating BIYAN QINGDU KELI is: get this product, add the hydrochloric acid solution heating in water bath and make dissolving, add 20% sodium hydroxide solution adjust pH to 11～12 again, put in the separatory funnel, add the ethyl acetate jolting and extract, standing demix, merge upper strata liquid, evaporate to dryness, residue add methanol makes dissolving as need testing solution; Other gets the Radix Zanthoxyli control medicinal material, added the hydrochloric acid solution heating in water bath 20 minutes, put coldly, filter, add 20% sodium hydroxide solution adjust pH to 11～12 again, put in the separatory funnel, add the ethyl acetate jolting and extract, standing demix merges upper strata liquid, evaporate to dryness, residue add methanol makes dissolving make control medicinal material solution; Test according to thin layer chromatography, draw above-mentioned need testing solution, control medicinal material solution, put respectively on same silica gel g thin-layer plate, it is in the expansion cylinder of developing solvent that lamellae is put with normal hexane-ethyl acetate-methanol-isopropyl alcohol-strong ammonia solution, presaturation 20 minutes launches, and takes out, dry, put under the ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
4, the method for quality control of a kind of BIYAN QINGDU KELI according to claim 1 is characterized in that the preferable condition of the gentiopicrin in the high effective liquid chromatography for measuring BIYAN QINGDU KELI is:
Assay is according to high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water is a mobile phase; Detect wavelength: 270nm; Number of theoretical plate calculates by the gentiopicrin peak should be not less than 3000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the gentiopicrin reference substance, adds 30% methanol and make the solution that every 1ml contains 40 μ g, promptly;
This product is got in the preparation of need testing solution, and porphyrize is got about 1g, accurate claims surely, puts in the 25ml volumetric flask, adds 30% methanol to nearly scale, and supersound process 10 minutes is put coldly, adds 30% methanol to scale, shakes up, and gets supernatant, promptly;
Accurate respectively reference substance solution and the need testing solution drawn of algoscopy injects chromatograph of liquid, measures, promptly; The every 1g of this product contains Radix Gentianae in gentiopicrin, must not be less than 0.5mg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200810029030XA CN101306139A (en) | 2008-06-26 | 2008-06-26 | Quality control method of Biyan Qingdu granule |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200810029030XA CN101306139A (en) | 2008-06-26 | 2008-06-26 | Quality control method of Biyan Qingdu granule |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101306139A true CN101306139A (en) | 2008-11-19 |
Family
ID=40122977
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA200810029030XA Pending CN101306139A (en) | 2008-06-26 | 2008-06-26 | Quality control method of Biyan Qingdu granule |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101306139A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101530463B (en) * | 2009-04-27 | 2013-01-02 | 中国科学院长春应用化学研究所 | Quality detection method of Chinese herb gentian |
| CN108693296A (en) * | 2018-05-23 | 2018-10-23 | 云南中丹红制药有限责任公司 | SHUMITONG JIAONANG and its raw material detection method |
-
2008
- 2008-06-26 CN CNA200810029030XA patent/CN101306139A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101530463B (en) * | 2009-04-27 | 2013-01-02 | 中国科学院长春应用化学研究所 | Quality detection method of Chinese herb gentian |
| CN108693296A (en) * | 2018-05-23 | 2018-10-23 | 云南中丹红制药有限责任公司 | SHUMITONG JIAONANG and its raw material detection method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102269751B (en) | Detection method of Liuweinengxiao preparation | |
| CN104161847A (en) | Quality detection method of traditional Chinese medicinal composition for curing diabetic retinopathy | |
| CN103808842B (en) | A kind of quality determining method of Chinese medicine preparation liver protection drip pill | |
| CN101829266A (en) | Method for detecting quality of bezoar snake bile bulbus fritilariae liquid | |
| CN102335402A (en) | Detection method of Chinese preparation mixture for invigorating the spleen and replenishing qi | |
| CN101982189A (en) | Method for detecting salvia heart-soothing capsules | |
| CN101264226B (en) | Quality detecting method of diabetes treating medicine | |
| CN102139039B (en) | Quality control method of coptis tablet for clearing away stomach heat | |
| CN102590431B (en) | Quality standard detection method for Chinese medicinal composition for treating cough | |
| CN104407092A (en) | Quality detection method of traditional Chinese medicinal composition with efficacy of appetizing and invigorating spleen | |
| CN101961472B (en) | Detection method for lung-soothing syrup | |
| CN101306139A (en) | Quality control method of Biyan Qingdu granule | |
| CN101897760A (en) | Detection method of Santanning syrup | |
| CN102552515A (en) | Quality detection method for blood-nourishing Chinese angelica syrup | |
| CN101780190B (en) | Detection method for pharmaceutic preparation containing sanguis draconis extract | |
| CN101317935B (en) | Rujietai formulation and quality detection method | |
| CN100543470C (en) | A kind of quality determining method of compound pyrrosia leaf particle | |
| CN1857445B (en) | Quality control method for Desheng preparation | |
| CN101979027A (en) | Method for detecting Jinze coronary disease capsules | |
| CN103675192A (en) | Detection method of inflammation-diminishing compound pierasma quassioides benn capsule | |
| CN104833756B (en) | A kind of content assaying method of attached sweet medicine monoester alkaloid | |
| CN111721855B (en) | Method for determining related substances of pharmaceutical preparation containing acetaminophen, dextromethorphan hydrobromide and doxylamine succinate | |
| CN103512999B (en) | The quality determining method of Fufang Huangqin Tablets by HPLC | |
| CN101112422A (en) | Quality control method of particles for eliminating phlegm and stopping cough for children | |
| CN102068599B (en) | Detection method for phlegm eliminating and asthma relieving cough syrup |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Open date: 20081119 |