CN104749311A - Method for examination of Sihuang dysentery-relieving particle quality - Google Patents
Method for examination of Sihuang dysentery-relieving particle quality Download PDFInfo
- Publication number
- CN104749311A CN104749311A CN201310739482.8A CN201310739482A CN104749311A CN 104749311 A CN104749311 A CN 104749311A CN 201310739482 A CN201310739482 A CN 201310739482A CN 104749311 A CN104749311 A CN 104749311A
- Authority
- CN
- China
- Prior art keywords
- solution
- yellow
- scutelloside
- control sample
- sample
- 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
- Nitrogen Condensed Heterocyclic Rings (AREA)
Abstract
The invention relates to a method for examination of Sihuang dysentery-relieving particle quality. The method is designed by proper improvement based on the original Sihuang dysentery-relieving particle standards and practical situation by product quality standard revision, adopts radix scutellariae identification and provides a berberine hydrochloride high performance liquid chromatography (HPLC) determination method. A methodology validation of the method proves that the method can effectively control product internal quality and guarantee product quality stability. The method has simple processes, satisfies traditional Chinese medicine product content determination requirements, controls active ingredient kinds as much as possible, improves a product quality level and improves market competitiveness.
Description
Technical field
The invention belongs to Chinese medicine detection technique field, relate to the method for a kind of inspection four yellow Zhili granule quality, the method can be used for carrying out comprehensive evaluation to four yellow Zhili granule quality.
Background technology
Four yellow Zhili granules are processed into after four yellow only dysentery medicinal extract by the coptis, golden cypress, rheum officinale, the Radix Astragali, Radix Isatidis, Radix Glycyrrhizae 6 taste Chinese medicine through extraction; the particle be mixed according to a certain percentage with sucrose, dextrin; there is effect of clearing heat-fire, only dysentery; the clinical treatment being mainly used in damp-heat dysentery and chicken colibacillosis, the damp-heat dysentery caused as the Escherichia coli of chicken, Pasteurella, salmonella infection and viral disease scabies secondary infection, dysentery characterized by white mucous stool, yellow-white dysentery, water sample rush down dysentery etc.; The serious spurting watery diarrhea etc. that the viral diseases such as swine escherichia coli, salmonellal diarrhoea, yellowish-white dysentery, transmissible gastroenteritis, epidemic diarrhea, rotavirus diarrhea cause.The curative effect definite because of it and good reputation, be included in People's Republic of China's veterinary drug allusion quotation 2010 editions 2 P587.
Quality control about four yellow Zhili granules only has " People's Republic of China's veterinary drug allusion quotation " 2010 editions two ministerial standards, wherein record: " more than four yellow Zhili granule [prescription] coptiss 200g golden cypress 200g rheum officinale 100g root of large-flowered skullcap 200g Radix Isatidis 200g Radix Glycyrrhizae 100g [method for making] 6 taste boiling 2 times; 2 hours first times; second time 1 hour; collecting decoction; filter; filtrate is concentrated into the thick paste that relative density is 1.32 ~ 1.35, add sucrose and dextrin is appropriate, make particle, drying, makes 1000g, to obtain final product.[proterties] this product is yellow to brown yellow granule.This product 10g is got in [discriminating] (1), adds zeyssatite 2.5g and grinds well, add methyl alcohol 50ml, and put in water-bath and reflux 1 hour, let cool, filter, filtrate is concentrated into 5ml as testing sample solution.Separately get coptis control medicinal material 2g, add methyl alcohol 20ml, be made in the same way of control medicinal material solution.Get Berberine hydrochloride reference substance again, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast.Test according to thin-layered chromatography (annex 32 pages), draw each 5 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with benzene-ethyl acetate-isopropanol-methyl alcohol-strong ammonia solution (6:3:1.5:1.5:0.5) for developping agent, put in the exhibition cylinder of ammonia saturated with vapor, presaturation 30 minutes, launch, take out, dry, inspect under putting uviol lamp (365nm).In testing sample chromatogram, with on control medicinal material chromatogram relevant position, show the fluorescence spot of same color; With on reference substance chromatogram relevant position, show an identical yellow fluorescence spot.(2) get this product 2g, add methyl alcohol 50ml, ultrasonic process 20 minutes, filter, filtrate evaporate to dryness, the residue 10ml that adds water makes dissolving, add hydrochloric acid 1ml again, put in water-bath and heat 30 minutes, cool immediately, extract at twice with ether, each 20ml, merges ether solution, water bath method, residue adds methenyl choloride 1ml makes dissolving, as testing sample solution.Separately get rheum officinale control medicinal material 0.1g, be made in the same way of control medicinal material solution.Test according to thin-layered chromatography (annex 32 pages), draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same with carboxymethylcellulose sodium solution be binder silica gel H thin layer plate on, with the upper solution of sherwood oil (30 ~ 60 DEG C)-ethyl formate-formic acid (15:5:1) for developping agent, launch, take out, dry, inspect under putting uviol lamp (365nm).In testing sample chromatogram, on the position corresponding to control medicinal material chromatogram, aobvious five identical orange-yellow fluorescence spots; Put after smoking in ammonia steam, spot becomes redness.
The thin-layer identification method of scutelloside and the HPLC content assaying method of Berberine hydrochloride, all have bibliographical information.
In " People's Republic of China's veterinary drug allusion quotation " 2010 editions two, the quality standard of four yellow Zhili granules is only differentiated the coptis and rheum officinale, other a few taste medicines are not all differentiated, assay item is not had yet, be unfavorable for controlling its quality, for ensure Clinical practice safety, effectively, stable, be necessary to set up a perfect quality inspection method.
Summary of the invention
Technical matters to be solved by this invention is for the deficiencies in the prior art, the method of a kind of inspection four yellow Zhili granule quality is provided, the method revises target level of product quality on the basis of four yellow Zhili granule primary standards, add the discriminating of the root of large-flowered skullcap, a kind of high performance liquid chromatography (HPLC) assay method of Berberine hydrochloride is provided simultaneously, more effectively can control the inherent quality of product, and ensure the stable of product quality.
For this reason, the invention provides the method for a kind of inspection four yellow Zhili granule quality, it comprises the discriminating of scutelloside and the assay of Berberine hydrochloride in four yellow Zhili granules.
According to the present invention, in described four yellow Zhili granules, the discriminating of scutelloside adopts thin-layered chromatography, and comprising with scutelloside is control sample, take methyl alcohol as solvent, respectively by control sample solution and four yellow Zhili granule testing sample extract solution point samples on same silica G plate, with ethyl acetate-butanone-formic acid-water for developping agent, be placed in exhibition cylinder after presaturation, expansion, take out, dry, spray with developer, and inspect.
If the result of inspecting is: show the spot with control sample same color in testing sample chromatogram on the position corresponding to control sample chromatogram, then illustrate in four yellow Zhili granule testing samples containing scutelloside.
According to the present invention, identify in the process of scutelloside in four yellow Zhili granules in employing thin-layered chromatography, the volume ratio of described developping agent ethyl acetate-butanone-formic acid-water is 5:3:1:1.
Compared with the developping agent adopting sherwood oil-ethyl formate-formic acid to form in thin-layer chromatographic analysis process with prior art, the developping agent of above-mentioned composition and proportioning thereof well can eliminate interference in thin-layer chromatographic analysis process, make principal spot degree of separation better.
In the present invention, term used " principal spot " refers to scutelloside spot, that is in testing sample chromatogram, on the position corresponding to control sample chromatogram, the spot of display and control sample same color.Compared with other impurity spots in testing sample, this spot is the strongest spot.
Term described in the present invention " is placed in and opens up presaturation in cylinder " presaturation referring to thin layer plate, refer to particularly before expansion, make developping agent steam saturated in expansion cylinder, expansion cylinder vapour-liquid state is made to reach certain steady state (SS), then putting into the thin layer plate that point sample is complete carries out saturated, and the thin layer plate Integral Differential opposite sex is reduced.The inferior separating effect that not good (as irregular in edge etc.) in thin layer plate preparation brings can be reduced like this, improve separating effect, and make spot correspondence more accurate.
Term described in the present invention " silica G plate " refers to the thin layer plate that the calcined gypsum adding 5% ~ 20% in silica gel obtains as bonding agent.
In the present invention, the silica G plate that above-mentioned silica gel g thin-layer plate is is binder with the carboxymethylcellulose sodium solution containing 4% sodium acetate.
In a specific embodiment of the present invention, identify in the process of scutelloside in four yellow Zhili granules in employing thin-layered chromatography, the concentration of described control sample solution is 1mg/ml.Described developer is 1% ferric trichloride ethanolic solution.The amount of described control sample solution and four yellow Zhili granule testing sample extract solution point samples is 5 μ l.The described presaturation time is 30min.
Adopt 1% ferric trichloride ethanolic solution to be that developer can contribute to sample colour developing, ethanol wherein can contribute to solvent volatilization.
In yet another embodiment of the present invention, described four yellow Zhili granule testing sample extract solutions are by the powder 14g of testing sample porphyrize, add methyl alcohol 50ml, ultrasonic process 20 minutes, to filter and by filtrate evaporate to dryness, then in residual residue, add 2ml methyl alcohol make it dissolve, elimination impurity obtains.
In one embodiment of the invention, thin-layered chromatography is adopted to differentiate scutelloside in four yellow Zhili granules: the powder 15g getting this product porphyrize, adds methyl alcohol 50ml, ultrasonic process 20 minutes, filters, filtrate evaporate to dryness, residue adds methyl alcohol 2ml makes dissolving, and filter, filtrate is as testing sample solution.Separately get scutelloside reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, sheet solution in contrast.Test according to thin-layered chromatography (annex 32 pages), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on the same silica G plate being binder with the carboxymethylcellulose sodium solution containing 4% sodium acetate, with ethyl acetate-butanone-formic acid-water (5:3:1:1) for developping agent, put presaturation 30 minutes in exhibition cylinder, launch, take out, dry, spray with 1% ferric trichloride ethanolic solution.In testing sample chromatogram, with on reference substance chromatogram relevant position, show the spot of same color.
According to the present invention, in described four yellow Zhili granules, the assay of Berberine hydrochloride adopts high performance liquid chromatography, comprise and adopt UV-detector and Agilent-C18 chromatographic column, take Berberine hydrochloride as control sample, with acetonitrile-potassium dihydrogen phosphate buffer solution for mobile phase, after reference substance solution and testing sample solution sample introduction, record chromatogram, with the content of external standard method by Berberine hydrochloride in the yellow Zhili granule of calculated by peak area four.
In an embodiment of the invention, the volume ratio of acetonitrile and potassium dihydrogen phosphate buffer solution is 30:70.The pH value of described buffer solution is 3.0.In described potassium dihydrogen phosphate buffer solution, the concentration of potassium dihydrogen phosphate is 0.05mol/L.
Term described in the present invention " potassium dihydrogen phosphate buffer solution " refers to water to be after solvent is mixed with the potassium dihydrogen phosphate aqueous solution of desired concn, then this solution is adjusted to the solution obtained by required pH value with hydrochloric acid.
In yet another embodiment of the present invention, the sample size of reference substance solution and testing sample solution is 20 μ l.
In the present invention, described control sample solution is made up of acetonitrile-aqueous solution, and in control sample solution, the concentration of Berberine hydrochloride is 0.1mg/ml, and in wherein said acetonitrile-aqueous solution, the volume ratio of acetonitrile and water is 3:7.
In one embodiment of the invention, adopt the content of high-performance liquid chromatogram determination Berberine hydrochloride, chromatographic condition is as follows:
Chromatographic column: octadecylsilane chemically bonded silica post, as Agilent-C18(150mm X4.6mm, 5 μm) etc.
Mobile phase: acetonitrile-0.05mol/L potassium dihydrogen phosphate buffer solution (with phosphoric acid adjust pH to 3.0) (30:70).
Flow velocity: 1ml/min; Determined wavelength: 265nm; Column temperature: 30 DEG C.
The preparation of reference substance solution: it is appropriate that precision takes Berberine hydrochloride reference substance, adds acetonitrile-water (3:7) mixed solution and makes the solution of every 1ml containing 0.1mg, to obtain final product.
Prepared by testing sample solution: get this product in right amount, porphyrize, gets 0.5g, accurately weighed, puts in 50ml measuring bottle, and add mobile phase appropriate, ultrasonic dissolution, is placed to room temperature, adds mobile phase and complements to scale, shake up, to obtain final product.
Determination method: accurate absorption reference substance solution and each 20 μ l of testing sample solution, injection liquid chromatography, record chromatogram, with external standard method by calculated by peak area, to obtain final product.
The method of the yellow Zhili granule quality of inspection four according to the present invention, suitably improve in conjunction with actual conditions on the basis of four yellow Zhili granule primary standards, carry out revision to target level of product quality to obtain, which increase the discriminating of the root of large-flowered skullcap, a kind of high performance liquid chromatography (HPLC) assay method of Berberine hydrochloride is provided simultaneously.The method, through Method validation, more effectively can control the inherent quality of product, and ensures the stable of product quality.The method is simple to operate, reaches the requirement of tcm product assay item and is controlled as much as possible effective constituent kind, the quality level of product is promoted, can increase the competitiveness of product in market.
Accompanying drawing explanation
Fig. 1 is control sample liquid chromatogram.
Fig. 2 is negative sample liquid chromatogram.
Fig. 3 is testing sample liquid phase chromatogram.
Embodiment
For making the present invention easier to understand, describe the present invention in detail below in conjunction with embodiment and accompanying drawing, these embodiments only play illustrative effect, are not limited to range of application of the present invention, NM specific experiment method in the following example, conveniently experimental technique carries out usually.
Embodiment
Embodiment 1:
1. the discriminating of the root of large-flowered skullcap:
Get the powder 14g of this product porphyrize, add methyl alcohol 50ml, ultrasonic process 20 minutes, filter, filtrate evaporate to dryness, residue adds methyl alcohol 2ml makes dissolving, and filter, filtrate is as testing sample solution.Separately get scutelloside reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast.Test according to thin-layered chromatography (annex 32 pages), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on the same silica G plate being binder with the carboxymethylcellulose sodium solution containing 4% sodium acetate, with ethyl acetate-butanone-formic acid-water (5:3:1:1) for developping agent, put presaturation 30 minutes in exhibition cylinder, launch, take out, dry, spray with 1% ferric trichloride ethanolic solution.In testing sample chromatogram, with on reference substance chromatogram relevant position, show the spot of same color.
2. the assay of Berberine hydrochloride:
(1) instrument reagent, sample
Instrument: Waterse2695 high performance liquid chromatograph; UV2489 UV-detector.
Reagent: second eyeball is chromatographically pure; Potassium dihydrogen phosphate is pure for analyzing; Water is secondary redistilled water.
Reference substance: Berberine hydrochloride is purchased from China Veterinery Drug Inspection Office.
Sample: be four yellow Zhili granules of our factory.
(2) chromatographic condition:
Chromatographic column: octadecylsilane chemically bonded silica post, as Agilent-C18(150mm X4.6mm, 5 μm) etc.
Mobile phase: acetonitrile-0.05mol/L potassium dihydrogen phosphate buffer solution (with phosphoric acid adjust pH to 3.0) (30:70).
Flow velocity: 1ml/min; Determined wavelength: 265nm; Column temperature: 30 DEG C.
(3) preparation of solution:
1. the preparation of reference substance solution: it is appropriate that precision takes Berberine hydrochloride reference substance, adds acetonitrile-water (3:7) mixed solution and makes the solution of every 1ml containing 0.1mg, to obtain final product.
2. testing sample solution preparation: get this product in right amount, porphyrize, gets 0.5g, accurately weighed, puts in 50ml measuring bottle, and add mobile phase appropriate, ultrasonic dissolution, is placed to room temperature, adds mobile phase and complements to scale, shake up, to obtain final product.
3. the preparation of negative sample: get the sample not adding the coptis, prepares by the preparation method of testing sample solution, measures by the chromatographic condition in 2.Negative sample chromatogram (see figure 2) and control sample chromatic graph are composed (see figure 1) and testing sample chromatic graph to compose (see figure 3) and compare visible, the position that Berberine hydrochloride peak occurs in reference substance collection of illustrative plates occurs there are no peak, shows that negative sample is noiseless.
(4) preparation of typical curve:
Get reference substance solution 5,10,20,30,50 μ l in 3 respectively, inject high performance liquid chromatograph, according to above-mentioned chromatographic condition, measure peak area.To contrast sample size for horizontal ordinate, with integrating peak areas value for ordinate, drawing standard curve, obtains regression equation.Result shows that Berberine hydrochloride is good in 0.513 ~ 5.260 μ g scope internal linear relation.
(5) precision test:
Get four yellow Zhili granule 1 part, by under 3 2. in method prepare test liquid, get test liquid 20 μ l, repeat sample introduction continuously 6 times by above-mentioned chromatographic condition, measure the content of Berberine hydrochloride, it is 1.12% that result records RSD.
(6) determination of recovery rates:
Get oneself and know four of content yellow Zhili granule 6 parts, every part of 0.25g, accurately weighed, respectively to wherein adding Berberine hydrochloride reference substance solution 10ml, by under 3 2. in method prepare test liquid, under above-mentioned chromatographic condition, measure content, calculate the recovery.Result average recovery rate is 100.1%, RSD is 1.77%.
As can be seen from above-described embodiment, the inventive method more effectively can control the inherent quality of product, and ensures the stable of product quality.The method is simple to operate, reaches the requirement of tcm product assay item and is controlled as much as possible effective constituent kind, the quality level of product is promoted, can increase the competitiveness of product in market.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. check a method for four yellow Zhili granule quality, it comprises the discriminating of scutelloside and the assay of Berberine hydrochloride in four yellow Zhili granules.
2. method according to claim 1, is characterized in that, in described four yellow Zhili granules, the discriminating of scutelloside adopts thin-layered chromatography, comprise with scutelloside is control sample, take methyl alcohol as solvent, respectively by control sample solution and four yellow Zhili granule testing sample extract solution point samples on same silica G plate, with ethyl acetate-butanone-formic acid-water for developping agent, to be placed in exhibition cylinder after presaturation, launch, take out, dry, spray with developer, and is inspected.
3. method according to claim 2, it is characterized in that, if the result of inspecting is: show the spot with control sample same color in testing sample chromatogram on the position corresponding to control sample chromatogram, then illustrate in four yellow Zhili granule testing samples containing scutelloside.
4. according to the method in claim 2 or 3, it is characterized in that, identify in the process of scutelloside in four yellow Zhili granules in employing thin-layered chromatography, the volume ratio of described developping agent ethyl acetate-butanone-formic acid-water is 5:3:1:1.
5. according to the method in claim 2 or 3, it is characterized in that, identify in the process of scutelloside in four yellow Zhili granules in employing thin-layered chromatography,
The concentration of described control sample solution is 1mg/ml;
Described developer is 1% ferric trichloride ethanolic solution;
The described presaturation time is 30min.
6. according to the method in claim 2 or 3, it is characterized in that, described four yellow Zhili granule testing sample extract solutions are by the powder 14g of testing sample porphyrize, add methyl alcohol 50ml, ultrasonic process 20 minutes, to filter and by filtrate evaporate to dryness, then in residual residue, add 2ml methyl alcohol make it dissolve, elimination impurity obtains.
7. method according to claim 1, it is characterized in that, in described four yellow Zhili granules, the assay of Berberine hydrochloride adopts high performance liquid chromatography, comprise and adopt UV-detector and Agilent-C18 chromatographic column, take Berberine hydrochloride as control sample, with acetonitrile-potassium dihydrogen phosphate buffer solution for mobile phase, after reference substance solution and testing sample solution sample introduction, record chromatogram, with the content of external standard method by Berberine hydrochloride in the yellow Zhili granule of calculated by peak area four.
8. method according to claim 7, is characterized in that,
The volume ratio of acetonitrile and potassium dihydrogen phosphate buffer solution is 30:70;
The pH value of described buffer solution is 3.0;
In described potassium dihydrogen phosphate buffer solution, the concentration of potassium dihydrogen phosphate is 0.05mol/L.
9. method according to claim 7, is characterized in that, the sample size of reference substance solution and testing sample solution is 20 μ l.
10. the method according to claim 7 or 9, it is characterized in that, described control sample solution is made up of acetonitrile-aqueous solution, and in control sample solution, the concentration of Berberine hydrochloride is 0.1mg/ml, and in wherein said acetonitrile-aqueous solution, the volume ratio of acetonitrile and water is 3:7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310739482.8A CN104749311A (en) | 2013-12-25 | 2013-12-25 | Method for examination of Sihuang dysentery-relieving particle quality |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310739482.8A CN104749311A (en) | 2013-12-25 | 2013-12-25 | Method for examination of Sihuang dysentery-relieving particle quality |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104749311A true CN104749311A (en) | 2015-07-01 |
Family
ID=53589305
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310739482.8A Pending CN104749311A (en) | 2013-12-25 | 2013-12-25 | Method for examination of Sihuang dysentery-relieving particle quality |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104749311A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110954645A (en) * | 2019-09-09 | 2020-04-03 | 山东琪康生物技术有限公司 | Detection method of high-quality Sihuang dysentery stopping granules |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01165391A (en) * | 1987-12-21 | 1989-06-29 | Seitai Kinou Riyou Kagakuhin Shinseizou Gijutsu Kenkyu Kumiai | Production of berberine type alkaloid |
| CN1538172A (en) * | 2003-04-17 | 2004-10-20 | 江苏康缘药业股份有限公司 | Quality control method for Chinese medicinal preparation |
| CN1803180A (en) * | 2005-01-13 | 2006-07-19 | 北京凯瑞创新医药科技有限公司 | Medicine composition and its preparation method and quality control method |
-
2013
- 2013-12-25 CN CN201310739482.8A patent/CN104749311A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01165391A (en) * | 1987-12-21 | 1989-06-29 | Seitai Kinou Riyou Kagakuhin Shinseizou Gijutsu Kenkyu Kumiai | Production of berberine type alkaloid |
| CN1538172A (en) * | 2003-04-17 | 2004-10-20 | 江苏康缘药业股份有限公司 | Quality control method for Chinese medicinal preparation |
| CN1803180A (en) * | 2005-01-13 | 2006-07-19 | 北京凯瑞创新医药科技有限公司 | Medicine composition and its preparation method and quality control method |
Non-Patent Citations (2)
| Title |
|---|
| 国家药典委员会: "《中华人民共和国药典2010版 一部》", 31 January 2010, article "桂林西瓜霜" * |
| 高靥: "芩连片质量控制方法与药物动力学研究", 《芩连片质量控制方法与药物动力学研究》, no. 11, 15 November 2008 (2008-11-15) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110954645A (en) * | 2019-09-09 | 2020-04-03 | 山东琪康生物技术有限公司 | Detection method of high-quality Sihuang dysentery stopping granules |
| CN110954645B (en) * | 2019-09-09 | 2020-09-29 | 山东琪康生物技术有限公司 | Detection method of high-quality Sihuang dysentery stopping granules |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102854281B (en) | Detection method of sugar-free strong loquat syrup | |
| CN102353732B (en) | Quality detection method of Zhenlong brain-refreshment preparation | |
| CN101703611B (en) | Quality detection method of Chinese angelica oral liquid for benefiting blood | |
| CN101204434A (en) | Quality standard for thrombus dispelling pill and test method thereof | |
| CN102218122A (en) | Quality control and detection method for sea dragon and gecko oral liquid | |
| CN103308644A (en) | Quality detection method for miscarriage-preventing leonurus preparation | |
| CN102068627A (en) | Quality control method for Chinese medicine preparation Xinnaojing tabelets | |
| CN103852555B (en) | A kind of quality determining method of Tibetan medicinal composition rheumatism Sialon preparation | |
| CN103344738B (en) | Detection method of nine-component heart-calming particle | |
| CN110954645B (en) | Detection method of high-quality Sihuang dysentery stopping granules | |
| CN102707006B (en) | Quality detection method of cudrania tricuspidata formula granules | |
| CN102331467B (en) | Method for detecting quality of south isatis root granules | |
| CN101703610A (en) | Quality detection method of Qingnao antihypertensive tablet | |
| CN104345117A (en) | Qualitative and quantitative detection method of compound Japanese Ardisia Herb tablets | |
| CN102198210B (en) | Quality control method of xiaojiean preparation | |
| CN104749311A (en) | Method for examination of Sihuang dysentery-relieving particle quality | |
| CN105806964A (en) | Method for detecting Acanthopanax senticosus and Glycyrrhiza uralensis preparation and application thereof | |
| CN103983735A (en) | Detection method for preparing Gongyanping (brand) capsules | |
| CN103575818B (en) | The blue or green granular mass control method of plate | |
| CN104569165B (en) | A kind of detection method peaceful for treating the treating coronary heart disease and angina pectoris compositions Ge Lan heart | |
| CN102854282B (en) | Detection method of traditional Chinese medicine compound preparation used for treating laryngopathy | |
| CN103512999B (en) | The quality determining method of Fufang Huangqin Tablets by HPLC | |
| CN102068599B (en) | Detection method for phlegm eliminating and asthma relieving cough syrup | |
| CN104764821A (en) | Method for determining content of active ingredients such as ephedrine hydrochloride and pseudoephedrine hydrochloride in asthma-relieving and cough-stopping syrup | |
| CN103901155B (en) | A kind of detection method for the treatment of the Chinese medicine composition of stomach trouble |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150701 |
|
| RJ01 | Rejection of invention patent application after publication |