CN102133268B - Quality control method of medicinal material - Google Patents
Quality control method of medicinal material Download PDFInfo
- Publication number
- CN102133268B CN102133268B CN 201010002653 CN201010002653A CN102133268B CN 102133268 B CN102133268 B CN 102133268B CN 201010002653 CN201010002653 CN 201010002653 CN 201010002653 A CN201010002653 A CN 201010002653A CN 102133268 B CN102133268 B CN 102133268B
- Authority
- CN
- China
- Prior art keywords
- peak area
- discrimination method
- rutin
- forsythoside
- 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.)
- Expired - Fee Related
Links
Images
Landscapes
- Saccharide Compounds (AREA)
Abstract
The invention, quality control method of medicinal material, discloses an identification method for distinguishing forsythia suspense medicinal materials processed by different methods; the identification method adopts high performance liquid chromatography for determination, uses a forsythiaside reference substance and a rutin reference substance as controls, determines the peak area of forsythiaside and the peak area of rutin, and calculates the ratio R of the peak area of forsythiaside and the peak area of rutin, wherein a value more than R represents eligibly processed forsythia suspense and a value less than R represents ineligibly processed forsythia suspense.
Description
Technical field
The present invention relates to a kind of method of quality control of medicinal material, particularly a kind of discrimination method of capsule of weeping forsythia medicinal material.
Background technology
The capsule of weeping forsythia is the dry fruit of the Oleaceae forsythia capsule of weeping forsythia [Forsythiasu spensor (Thunb) va hl].It is long avette to avette that the capsule of weeping forsythia is, and long 1.5-2 centimetre, diameter 0.5-1.3 centimetre.There is the fleck of irregular vertical wrinkle and most projectioies on the surface, and respectively there is a tangible longitudinal furrow on the two sides, and the sharp point in top, base portion have little carpopodium or come off.The capsule of weeping forsythia divides green grass or young crops to stick up and sticks up (Huang sticks up) always, and green grass or young crops sticks up with sticking up always because collecting time is different with job operation and forms.Green grass or young crops sticks up and is 8-9 before White Dew days immature dark green fruits still of gathering, and after boiling a moment or steam 30 minutes with cage with boiling water, takes out and dries into green grass or young crops and stick up.How green grass or young crops does not ftracture if sticking up, surperficial green and brown look, and the canescence fleck of projection is less, and matter is hard, the seed majority, yellow green, an elongated side have wing.Stick up always and be fruit maturation after the Frost's Descent in October, pericarp flavescence brown is taken when fruit splits, and removes seed for sticking up always.Stick up from top cracking always or be cleaved into two lobes, surperficial yellowish-brown or rufous, it is fallow that inside surface mostly is, level and smooth, tool one mediastinum.Matter is crisp, and seed is brown, how to come off.
Pharmacological actions such as that the capsule of weeping forsythia has is antibiotic, cardiac stimulant, diuresis, town are told, diseases such as the acute anemopyretic cold of forsythia fruit for treating commonly used, carbuncle sore tumefacting virus, scrofula, urinary tract infections.The capsule of weeping forsythia is the primary raw material of Chinese medicine preparations such as 'Shuang Hualian ', heat-clearing and detoxicating oral liquid, the careless analgesic oral liquid of company, flos ionicerae and fructus forsythiae infusion for detoxication.
In 'Shuang Hualian ', the proportionate relationship of the three flavor bulk drug capsules of weeping forsythia, honeysuckle, the root of large-flowered skullcap is 2: 1: 1, the consumption maximum of the capsule of weeping forsythia, and in the side capsule of weeping forsythia can removing summer-heat lung channel hot and suffocating, the wind-heat that can gently declare lung to defend again, have the merit of " clearing heat and detoxicating heresy " (" science of Chinese materia medica "), be monarch drug in a prescription, so the capsule of weeping forsythia raw material of ensuring the quality of products stable is to guarantee the stay-in-grade prerequisite of 'Shuang Hualian ' and basis.
'Shuang Hualian ' comprises granule, lozenge, dispersing tablet, chewable tablets, effervescent tablet, oral liquid, eye drops, aerosol, capsule, soft capsule, suppository, injection and powder-injection.State Food and Drug Administration in 2009 carries out the traditional Chinese medicine security and revalues work, purpose is to control the security risk of the traditional Chinese medicine that goes on the market, guarantee that the public is safe and effective for medication, wherein explicitly call for the quality control to raw material, basic former, the medicinal part, the place of production, picking time, place of production processing, the storage requirement that comprise fixing medicinal material, set up metastable medicinal material base, set up the strong injection of controllability raw material quality standard, improve quality control project etc.
The present invention carried out the injection security just and revalues under the background of work in 2009, the capsule of weeping forsythia medicinal material of different concocting process is carried out the research of discrimination method, for the first time breakthrough a kind of novelty of proposition, clearly, the green grass or young crops that different concocting process are distinguished in feasible discriminating sticks up, the method of quality control that sticks up always and control criterion, thereby set up the raw material quality standard of the strong 'Shuang Hualian ' injection agent of controllability, the perfect quality control project of capsule of weeping forsythia medicinal material, guarantee the steady quality of capsule of weeping forsythia medicinal material, thereby reduce the security risk of Chinese medicine 'Shuang Hualian ' injection agent, guarantee the steady quality of 'Shuang Hualian ' injection agent, controlled.
Summary of the invention
The discrimination method that provides a kind of green grass or young crops of distinguishing different concocting methods to stick up, stick up always is provided the object of the invention.
Discrimination method of the present invention is as follows:
Adopt high effective liquid chromatography for measuring, be contrast with Forsythoside reference substance, control substance of Rutin, by measuring Forsythoside peak area, rutin peak area, calculate Forsythoside peak area and rutin peak area ratio R, be limited with the R value, greater than sticking up for concocting qualified green grass or young crops of R value, less than sticking up for sticking up always or concocting underproof green grass or young crops of R value.
R value of the present invention is defined as 18, R value and is preferably 20.
The concrete preferred discrimination method of the present invention is as follows:
Chromatographic condition and system suitability test are filling agent with the octadecylsilane chemically bonded silica; With methyl alcohol-glacial acetic acid aqueous solution, or methyl alcohol-acetonitrile-glacial acetic acid aqueous solution is carried out wash-out for the phase that flows; The detection wavelength is 278nm.
The Forsythoside reference substance is got in the preparation of reference substance solution, control substance of Rutin is an amount of, adds 30-100% methyl alcohol and dissolves respectively, namely.
The preparation of need testing solution gets respectively that decatize green grass or young crops sticks up, poach green grass or young crops sticks up, sun-dried green grass or young crops sticks up and stick up pulverizing medicinal materials always, and the powder 1g that gets it filled adds methyl alcohol 30-50ml, and ultrasonic extraction is filtered, namely.
Determination method is accurate reference substance solution and each 5～20 μ l of need testing solution of drawing respectively, injects liquid chromatograph, measures.
Calculate Forsythoside peak area and rutin peak area ratio R in the different test sample chromatograms.
Wash-out of the present invention is gradient or isocratic elution, and the time of wash-out is 30 minutes-90 minutes, preferred 30 minutes-50 minutes; The ratio of methyl alcohol is 15%-45% in flowing mutually, preferred 25%-40%; The ratio of acetonitrile is 0-20%, preferably 0-10%; The ratio of glacial acetic acid aqueous solution is 55%-85%, preferred 60%-75%; The concentration of glacial acetic acid aqueous solution is greater than 0.1%.
The present invention definition greater than the R value for decatize green grass or young crops sticks up, poach green grass or young crops sticks up, or the green grass or young crops of the qualified regulation of other concocting method gained sticks up, less than the R value for stick up always, sun-dried green grass or young crops sticks up or the underproof green grass or young crops of other concocting methods sticks up.
Discrimination method of the present invention can effectively be distinguished the poach of different concocting methods, the green grass or young crops of decatize sticks up, and sun-dried green grass or young crops sticks up and sticks up always, thereby reaches the purpose of control product quality.This discrimination method mainly is by finding specific, sensitive R value, can isolating the capsule of weeping forsythia medicinal material of different concocting methods accurately.Simultaneously, the present invention by a large amount of experiment confirm when R value during greater than the numerical value in interval necessarily, the Chinese medicine preparation medicinal material that identifies is qualified, and the medicinal raw material that is lower than the R value of certain interval numerical value does not all meet the requirement of Chinese medicine preparation method, especially do not meet the ingredient requirement of Chinese medicine 'Shuang Hualian ' injection agent, therefore by discrimination method of the present invention, can guarantee the steady quality of capsule of weeping forsythia medicinal material, thereby reduce the security risk of Chinese medicine 'Shuang Hualian ' injection agent, the steady quality of assurance 'Shuang Hualian ' injection agent, controlled.
Discrimination method degree of separation of the present invention, stability, repeatability and the recovery are all better, degree of separation R＞1.0; In the stability test, Forsythoside peak area RSD is 0.39%, and rutin peak area RSD is 2.5%, and forsythin peak area RSD is 1.3%; In the replica test, Forsythoside peak area RSD is 0.98%, and rutin peak area RSD is 0.64%, and forsythin peak area RSD is 1.4%; The Forsythoside peak area that the green grass or young crops of poach or decatize sticks up and the ratio of rutin peak area, with stick up always the ratio of Forsythoside peak area and rutin peak area, P has statistical significance less than 0.05.
Description of drawings
Fig. 1 Forsythoside reference substance HPLC figure.
Fig. 2 control substance of Rutin HPLC figure.
Fig. 3 green grass or young crops sticks up (lot number Y070601) HPLC figure, and No. 1 peak is the Forsythoside peak, and No. 2 peaks are the rutin peak.
Fig. 4 sticks up (lot number Y091004) HPLC figure always, and No. 1 peak is the Forsythoside peak, and No. 2 peaks are the rutin peak.
Experimental example 1: flow and investigate experiment mutually
(1) flow and to have investigated methyl alcohol-0.1% glacial acetic acid aqueous solution mutually and see the following form 1:
(2) flow and to have investigated methyl alcohol-acetonitrile-0.1% glacial acetic acid aqueous solution mutually and see the following form 2:
(3) flow and to have investigated methyl alcohol-acetonitrile-0.1% glacial acetic acid aqueous solution mutually and see the following form 3:
The result shows that condition (1), (2) all can make Forsythoside, rutin, forsythin reach baseline separation, but the mobile phase chromatographic peak degree of separation that technical solution of the present invention is selected for use is bigger, and condition (3) Forsythoside can not reach baseline separation;
Experimental example 2: the investigation experiment of extracting solvent volume
Get the capsule of weeping forsythia medicinal powder 1g that pulverized 40 mesh sieves, three parts, put respectively in the 100ml conical flask, add 30ml, 40ml, 50ml methyl alcohol (sample 1, sample 2, sample 3) respectively, weigh, put coldly behind the ultrasonic 1h, weigh, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, the accurate subsequent filtrate of drawing, measure by above-mentioned chromatographic condition, the record chromatogram the results are shown in Table 4,5.
Table 4 extracts solvent and investigates the result
Table 5 extracts solvent and investigates interpretation of result
According to above-mentioned experimental result, the preferred 40ml methyl alcohol of the present invention extracts.
Experimental example 3: the investigation experiment of extraction time
Get the capsule of weeping forsythia medicinal powder 1g that pulverized 40 mesh sieves, three parts, put respectively in the 100ml conical flask, add 40ml methyl alcohol ultrasonic 30min respectively, 40min is put cold (sample 1 behind the 50min, sample 2, sample 3), weigh, supply the weight that subtracts mistake with methyl alcohol, filter, the accurate subsequent filtrate of drawing is measured by above-mentioned chromatographic condition, the record chromatogram the results are shown in Table 6.
Table 6 extraction time investigation result
According to above-mentioned experimental result, the preferred ultrasonic time of the present invention is 40min.
Following embodiment is used for further specifying but is not limited to the present invention.
Embodiment 1: the liquid phase that green grass or young crops sticks up is differentiated
Instrument: U.S.'s Agilent 1100 high performance liquid chromatographs/U.S.'s Agilent 1200 high performance liquid chromatographs (VWD detecting device, ChemStation for LC chromatographic work station); Agilent ZORBAX Eclipse XDB-C18 chromatographic column (4.6 * 250mm, C184.6 * 10mm guard column); Plum Teller-Tuo benefit AB135-S electronic balance.
Reagent: forsythin reference substance (Nat'l Pharmaceutical ﹠ Biological Products Control Institute's lot number: 110821-200711), control substance of Rutin (Nat'l Pharmaceutical ﹠ Biological Products Control Institute's lot number: 100080-200707), (medical sci-tech Development Co., Ltd is merged in Shanghai provides lot number to the Forsythoside chemical reference substance: 090923); Acetonitrile (chromatographically pure), methyl alcohol (chromatographically pure), glacial acetic acid (analyzing pure), water (self-control ultrapure water).
Chromatographic condition and system suitability test are filling agent with the octadecylsilane chemically bonded silica; With methyl alcohol-0.1% glacial acetic acid aqueous solution, or methyl alcohol-acetonitrile-0.1% glacial acetic acid aqueous solution is carried out gradient elution for the phase that flows; The detection wavelength is 278nm; Forsythoside, rutin, the forsythin degree of separation is all greater than 1.
The Forsythoside reference substance is got in the preparation of reference substance solution, and control substance of Rutin is an amount of, adds 30-70% methyl alcohol and dissolves respectively and make the solution that every 1ml contains 0.05mg/ml, namely.
The preparation of need testing solution is got green grass or young crops and is stuck up pulverizing medicinal materials, oven dry, and the powder 1g that gets it filled adds methyl alcohol 40ml, weighs, and puts coldly behind the ultrasonic 40min, weighs, and supplies the weight that subtracts mistake with methyl alcohol, shakes up, and filters, namely.
Determination method is accurate reference substance solution and each 5 μ l of need testing solution of drawing respectively, injects liquid chromatograph, measures.
Calculate the ratio of Forsythoside peak area and rutin peak area in the different samples, the Forsythoside peak area that green grass or young crops sticks up and the ratio of rutin peak area should be less than 18, the results are shown in Table 7, Fig. 3 [green grass or young crops sticks up (lot number Y070601) HPLC chromatogram].
Table 7 green grass or young crops sticks up the sample determination result
| Sequence number | The sample name | The sample lot number | The sample concocting method | The Forsythoside area | The rutin area | Ester glycosides area/ |
| 1 | Green grass or young crops sticks up | Y070102 | The heated kang oven dry | 5878 | 309 | 19.0 |
| 2 | Green grass or young crops sticks up | Y070302 | Gas steams oven dry | 8266 | 317 | 26.1 |
| 3 | Green grass or young crops sticks up | Y070303 | Gas steams oven dry | 6793.8 | 265.2 | 25.6 |
| 4 | Green grass or young crops sticks up | Y070601 | Gas steams oven dry | 6031.9 | 217.2 | 27.8 |
| 5 | Green grass or young crops sticks up | Y070901 | Gas steams oven dry | 4106.9 | 191.9 | 21.4 |
| 6 | Green grass or young crops sticks up | Y071002 | The poach oven dry | 8049.1 | 332.1 | 24.2 |
| 7 | Green grass or young crops sticks up | Y091001 | Gas steams oven dry | 5523.8 | 245.3 | 22.5 |
| 8 | Green grass or young crops sticks up | Y080101 | Gas steams oven dry | 7885 | 333.7 | 23.6 |
| 9 | Green grass or young crops sticks up | Y080501 | The poach oven dry | 6551.1 | 304.8 | 21.5 |
| 10 | Green grass or young crops sticks up | Y091002 | Sun-dried | 1638 | 128.4 | 12.8 |
| 11 | Green grass or young crops sticks up | Y070102 | Sun-dried | 1227.9 | 141.2 | 8.7 |
Embodiment 2: the liquid phase of sticking up is always differentiated
Measure according to embodiment 1 method and to stick up sample always, record Forsythoside peak area, rutin peak area, the area ratio of Forsythoside and rutin in the calculation sample the results are shown in Table 8, Fig. 4 [sticking up (lot number Y091004) HPLC chromatogram always].
Table 8 sticks up the sample determination result always
| The sample name | The sample lot number | The sample concocting method | The Forsythoside area | The rutin area | Ester glycosides area/ |
|
| 1 | Stick up always | Y091014 | Dry | 469.2 | 41.7 | 11.3 |
| 2 | Stick up always | Y091015 | Dry | 509.4 | 44 | 11.6 |
| 3 | Stick up always | Y091003 | Dry | 281.1 | 38.4 | 7.3 |
| 4 | Stick up always | Y091016 | Dry | 137.6 | 72.5 | 1.9 |
| 5 | Stick up always | Y091004 | Dry | 413.1 | 72.6 | 5.7 |
[0062]
| 6 | Stick up always | Y091017 | Dry | 26.9 | 0 | - |
| 7 | Stick up always | Y091005 | Dry | 467.9 | 48.8 | 9.6 |
| 8 | Stick up always | Y091018 | Dry | 1069.8 | 72.5 | 14.8 |
| 9 | Stick up always | Y091006 | Dry | 249.9 | 42.1 | 5.9 |
| 10 | Stick up always | Y091007 | Dry | 76 | 30.6 | 2.5 |
| 11 | Stick up always | Y091008 | Dry | 381.4 | 58.1 | 6.6 |
| 12 | Stick up always | Y091009 | Dry | 215.8 | 57.3 | 3.8 |
| 13 | Stick up always | Y091010 | Dry | 134.9 | 42 | 3.2 |
| 14 | Stick up always | Y091011 | Dry | 225.5 | 42.1 | 5.4 |
| 15 | Stick up always | Y091012 | Dry | 191.9 | 29.3 | 6.5 |
| 16 | Stick up always | Y091013 | Dry | 146 | 47.2 | 3.1 |
Claims (7)
1. the discrimination method of a capsule of weeping forsythia medicinal material, it is characterized in that this discrimination method adopts the special highly effective liquid chromatography for measuring, be filling agent with the octadecylsilane chemically bonded silica, be the phase that flows with methyl alcohol-0.1% glacial acetic acid aqueous solution or methyl alcohol-acetonitrile-0.1% glacial acetic acid aqueous solution, wherein, the ratio of methyl alcohol is 25%-40%; The ratio of acetonitrile is 0-10%, and the ratio of 0.1% glacial acetic acid aqueous solution is 60%-75%; The detection wavelength is 278nm; Be contrast with Forsythoside reference substance, control substance of Rutin, by measuring Forsythoside peak area, rutin peak area, calculate Forsythoside peak area and rutin peak area ratio R, greater than sticking up for concocting qualified green grass or young crops of R value, less than sticking up for sticking up always or concocting underproof green grass or young crops of R value.
2. discrimination method as claimed in claim 1 is characterized in that the R value is 18 in this discrimination method.
3. discrimination method as claimed in claim 1 or 2 is characterized in that being prepared as of reference substance solution in this discrimination method got the Forsythoside reference substance, control substance of Rutin is an amount of, adds 30-100% methyl alcohol and dissolves respectively, namely.
4. discrimination method as claimed in claim 1 or 2 is characterized in that the capsule of weeping forsythia pulverizing medicinal materials of getting different concocting methods respectively that is prepared as of need testing solution in this discrimination method, and the powder 1g that gets it filled adds methyl alcohol 30-50ml, and ultrasonic extraction is filtered, namely.
5. discrimination method as claimed in claim 1 or 2 is characterized in that in this discrimination method:
The experiment of chromatographic condition and system suitability: being filling agent with the octadecylsilane chemically bonded silica, be mobile phase with methyl alcohol-0.1% glacial acetic acid aqueous solution, and its elution requirement is as follows:
Accurate reference substance solution and each 5-20ul of need testing solution of drawing injects liquid chromatograph respectively, measures; Calculate Forsythoside peak area and rutin peak area ratio R in the different test sample chromatograms.
6. discrimination method as claimed in claim 1 or 2 is characterized in that in this discrimination method:
The experiment of chromatographic condition and system suitability: being filling agent with the octadecylsilane chemically bonded silica, be mobile phase with methyl alcohol-acetonitrile-0.1% glacial acetic acid aqueous solution, and its elution requirement is as follows:
Accurate reference substance solution and each 5-20ul of need testing solution of drawing injects liquid chromatograph respectively, measures;
Calculate Forsythoside peak area and rutin peak area ratio R in the different test sample chromatograms.
7. as claim 5 or 6 described discrimination methods, the R value is the capsule of weeping forsythia medicinal material that decatize green grass or young crops sticks up, poach green grass or young crops sticks up or can use as raw material greater than 18 capsule of weeping forsythia medicinal material in this discrimination method, R value less than 18 for stick up always, sun-dried green grass or young crops sticks up or other concocting method gained can not be as the capsule of weeping forsythia medicinal material of raw material use.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010002653 CN102133268B (en) | 2010-01-21 | 2010-01-21 | Quality control method of medicinal material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010002653 CN102133268B (en) | 2010-01-21 | 2010-01-21 | Quality control method of medicinal material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102133268A CN102133268A (en) | 2011-07-27 |
| CN102133268B true CN102133268B (en) | 2013-08-28 |
Family
ID=44293281
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010002653 Expired - Fee Related CN102133268B (en) | 2010-01-21 | 2010-01-21 | Quality control method of medicinal material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102133268B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107271594B (en) * | 2017-07-14 | 2019-09-17 | 河南中大恒源生物科技股份有限公司 | A method of identifying Natural Curcumin and synthesis curcumin |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1385412A (en) * | 2002-06-07 | 2002-12-18 | 牛勃 | Method for extracting hypericin from Hypericum perforatum and medicine made up using hypericin as main composition |
-
2010
- 2010-01-21 CN CN 201010002653 patent/CN102133268B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1385412A (en) * | 2002-06-07 | 2002-12-18 | 牛勃 | Method for extracting hypericin from Hypericum perforatum and medicine made up using hypericin as main composition |
Non-Patent Citations (1)
| Title |
|---|
| 吴艳芳,等.伏牛山区青翘与老翘药材质量的检测.《时珍国医国药》.2009,第20卷(第5期),1129-1130. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102133268A (en) | 2011-07-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103330758A (en) | Peony and liquorice soup formula granule, preparation method and detection method of peony and liquorice soup formula granule | |
| CN104161847B (en) | A kind of quality determining method of the Chinese medicine composition treating diabetic retinopathy | |
| CN105758985B (en) | A kind of quality determining method of virgin health piece | |
| CN103197027A (en) | Quality control method of astragalus-leech capsules capable of regulating collaterals | |
| CN114689774B (en) | Preparation process and quality control method of standard decoction of radix angelicae sinensis blood replenishing decoction | |
| CN106093262A (en) | A kind of method of the finger printing of the pharmaceutical preparation setting up Radix Scrophulariae | |
| CN102274401B (en) | Traditional Chinese medicine preparation for treating gastropathy and preparation method and detection method thereof | |
| CN102590212B (en) | Detection method of Jiuwei Zhuhuang preparation | |
| CN104391072A (en) | Quality control method of traditional Chinese medicine compound preparation for treating osteoporosis | |
| CN101879270A (en) | Chinese medicinal injectable powder and quality control method thereof | |
| CN102645493B (en) | Detection method of Wuweiganlu preparation | |
| CN102890124A (en) | Fingerprint constructing method of total flavonoid components and total alkaloids components in loranthus parasiticus-kudzuvine root preparation and quality detecting method | |
| CN101187651B (en) | Detection method of tongsaimai formualtion | |
| CN104792889A (en) | Flos lonicerae and radix scutellariae lung-clearing preparation fingerprint spectrum establishment method and standard fingerprint spectrum and application thereof | |
| CN102133268B (en) | Quality control method of medicinal material | |
| CN101816753B (en) | Method for detecting quality of compound preparation for treating cold | |
| CN104069200A (en) | "Sanhuang" heart-fire removing decoction formula granules and preparing method and detection method thereof | |
| CN103123343B (en) | Quality control method for Songling Xuemaikang capsules | |
| CN107607653A (en) | The method for determining Radix Scrophulariae extract finger-print | |
| CN108535399A (en) | A kind of detection method of Fuyankang pill | |
| CN104458954B (en) | A kind of dodder formulation granule finger printing and method for building up thereof | |
| CN107389827A (en) | The assay method of stachydrine hydrochloride content in motherwort or its compound preparation | |
| CN103760271B (en) | The detection method of brain heart clearing capsule | |
| CN103134896A (en) | Detection method for Chinese materia medica preparation for treating chronic prostatitis | |
| CN101953978A (en) | Heart-soothing and lipid-lowering tablet medicine quality standard detecting method |
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 | ||
| DD01 | Delivery of document by public notice | ||
| DD01 | Delivery of document by public notice |
Addressee: Heilongjiang Songhuajiang Pharmaceutical Co., Ltd. Document name: Notification of Termination of Patent Right |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130828 Termination date: 20180121 |