CN101936974B - Method for identifying Chinese patent drugs by using mixed contrast - Google Patents
Method for identifying Chinese patent drugs by using mixed contrast Download PDFInfo
- Publication number
- CN101936974B CN101936974B CN 201010221934 CN201010221934A CN101936974B CN 101936974 B CN101936974 B CN 101936974B CN 201010221934 CN201010221934 CN 201010221934 CN 201010221934 A CN201010221934 A CN 201010221934A CN 101936974 B CN101936974 B CN 101936974B
- Authority
- CN
- China
- Prior art keywords
- contrast
- test sample
- chinese patent
- chromatogram
- flavor
- 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
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention relates to a method for identifying on Chinese patent drugs by using mixed contrast, which comprises the steps of: 1, obtaining a supply sample chromatogram map; 2, obtaining a mixed contrast chromatogram map; and 3, comparing whether retention times of chromatographic peaks in the supply sample chromatogram map and the mixed contrast chromatogram map are consistent or not. The invention has the advantages of identifying drug tastes of the Chinese patent drugs by using a supply sample contrast mode under the same chromatogram condition, overcoming the bottleneck problem of identifying the drugs only by the conventional Chinese patent drug quality standard, controlling the integral quality of the drugs, and greatly saving detection time and cost.
Description
Technical field
The present invention relates to a kind of the utilization and mix the method that contrast is differentiated Chinese patent drug.
Background technology
The quality assessment of Chinese medicine is an insoluble difficult point problem always, and saying of " pill, powder, extract and pellet, angle's difficulty is distinguished " arranged from ancient times, and from founding of New till now, traditional Chinese medicine quality has also been realized by control to the transition of check control afterwards with the process experience.In recent years, along with the modern chemical analysis continuous advancement in technology, research means and the method for the inherent chemical constitution of Chinese patent drug are more and more, known inherent composition and assay method thereof are used for quality control, formulate corresponding test stone, very much progress has been arranged, the Chinese crude drug that records as Chinese Pharmacopoeia version in 1963 has only Ji Yuan and outward appearance shape to differentiate, Chinese patent drug then only has prescription and method for making, without any Interventions Requested.Version had then adopted micro-discriminating in a large number in 1977, and since 1985 editions pharmacopeia, chromatogram, spectral technique are used in traditional Chinese medicine quality control in a large number, and the Chinese patent drug that version pharmacopeia in 2005 is recorded assay just has 720 kinds.But the continuous increase along with the Chinese patent drug test item; round of visits is more and more longer; the poisonous and harmful reagent that uses is also more and more; as detoxicating tablet of cow-bezoar that records of Chinese Pharmacopoeia version in 2010 4 discriminatings are arranged; 1 content, Liuwei Dihuang Wan have recorded 6 discriminatings, 2 content; the round of visits of these medicines all needs to use poisonous and harmful reagent to reach 6～10 kinds more than 1 week.Moreover Chinese medicine is done as a whole, and what emphasize is diagnosis and treatment based on an overall analysis of the illness and the patient's condition, and what emphasize is the synergy of medicine of respectively distinguishing the flavor of, and the control of single active ingredient or index components in the Chinese patent drug at present is difficult to really control drug quality.Some pharmaceutical factory is in order to reduce cost, utilize the medicine inspection quality standard can not control the leak of all flavour of a drug fully, illegal production, do not feed intake or feed intake less for some flavour of a drug that can't check, feed intake for the flavour of a drug that assay is arranged more, make the Chinese patent drug curative effect be difficult to guarantee, people's health is caused grave danger, and medicine inspection department is difficult to also detect.Finger-print contains compounding substances group's method of quality control as Chinese patent drug, this class of herb extracts in this case, has become present international consensus.But present stage finger-print research is in the starting period, the finger-print of simple relatively parenteral solution is formed in main research, its reason mainly is that the fingerprint collection of illustrative plates is subjected to the medicinal material place of production, processing, experimental situation, factor affecting such as chromatographic condition are bigger, poor reproducibility between each laboratory is difficult to promote, and some common Chinese patent drugs can't employing fingerprint collection of illustrative plates control quality.
Summary of the invention
Technical matters to be solved by this invention provides a kind of the utilization and mixes the method that contrast is differentiated Chinese patent drug.
The technical solution adopted for the present invention to solve the technical problems:
Concrete steps of the present invention are as follows:
(1) obtain the test sample chromatogram:
A: take by weighing test sample;
B: preparation need testing solution;
The extracting method of selecting to adapt according to the character of the contained chemical constitution of crude drug of respectively distinguishing the flavor of in the described test sample prepares need testing solution;
C: select the chromatographic condition that adapts according to the character of the contained chemical analysis of crude drug of respectively distinguishing the flavor of in the described test sample, test is record test sample chromatogram also;
(2) obtain mixing contrast color spectrogram:
Described mixing contrast refers to get the product of control medicinal material in prescription ratio mixing gained of respectively distinguishing the flavor of in the described test sample;
A: take by weighing and mix contrast with described test sample equivalent described;
B: preparation mixes contrast solution: the preparation of preparation method and process conditions and described need testing solution is identical;
C: under the same chromatographic condition in going on foot with above-mentioned (1), test and record described mixing contrast color spectrogram;
(3) whether each chromatographic peak retention time is consistent in contrast test sample chromatogram and the mixing contrast color spectrogram.
The instrument that test color spectrogram of the present invention adopts comprises high performance liquid chromatograph, gas chromatograph, Ultra Performance Liquid Chromatography instrument and liquid chromatography mass combined instrument, gas chromatograph-mass spectrometer.Beneficial effect of the present invention is as follows:
(1) the present invention has introduced " mixing contrast " this completely new concept, adopts the mixing control medicinal material to combine with Modern Instrument Analytical Technique, and the gained chromatogram contains much information.
(2) utilize to mix normal control mode can be under same chromatographic condition to Chinese patent drug in each flavour of a drug differentiate, overcome the bottleneck problem that conventional Chinese patent drug quality standard is only differentiated a few flavor medicines wherein, not only can control the medicine total quality, and save proving time and cost greatly.
(3) the present invention takes to mix control medicinal material and test sample is measured under same experiment condition, has overcome the restriction of finger-print to chromatographic column, instrument, is easy to apply.
(4) it is many to the invention solves existing standard for traditional Chinese medicines discriminating project, method is numerous tired, problems such as poisonous and harmful reagent use amount is big, solved especially existing standard under the situation that consumes a large amount of artificial and reagent, can not control fully medicine quality this be stranded a difficult problem of scratching the Chinese patent drug development for a long time, can be widely used in during Chinese patent drug quality control, new Chinese medicine develop.
Description of drawings
Fig. 1 is storax pill for treating coronary heart disease mixing contrast color spectrogram.
Fig. 2 is storax pill for treating coronary heart disease test sample chromatogram.
The anti-asthma pill mixing contrast color spectrogram of coughing till Fig. 3.
The anti-asthma pill test sample chromatogram of coughing till Fig. 4.
Embodiment
Embodiment 1 (utilizing the gas chromatography mass spectrometry technology that each flavour of a drug in the storax pill for treating coronary heart disease are differentiated):
Storax pill for treating coronary heart disease is made up of borneol, frankincense, santal, storax, elecampane five tastes medicinal material, has the wide chest of regulating the flow of vital energy, and the effect of pain relieving is clinical in angina pectoris, uncomfortable in chest, treatment of conditions such as feel suffocated.
(1) key instrument: gas chromatograph-mass spectrometer (Shimadzu 2010Plus, Japan), balance (Metters AE-163, Switzerland).
(2) material and reagent: borneol, frankincense, santal, storax, elecampane control medicinal material (middle inspection institute, lot number: 110743-200504,120970-200604,121240-200402,120931-200202,121090-200602).
The test sample storax pill for treating coronary heart disease is available from pharmacy.
Water is pure water, and it is pure that other reagent is analysis.
(3) chromatographic condition: chromatographic column: Rtx-5ms fused-silica capillary column (30m * 0.25mm * 0.25 μ m); Temperature programme: 80 ℃ kept 4 minutes, rose to 120 ℃ with 10 ℃/min, were raised to 280 ℃ with 15 ℃/min again, kept 3min; Injector temperature: 250 ℃; Carrier gas is He gas, carrier gas flux 1.2mL/min; Sample size: 1 μ L; Split ratio is 20: 1.
(4) mass spectrum condition: ion gun is the EI source; Ion source temperature: 230 ℃; Interface temperature: 280 ℃; Sweep limit 50～400amu; Solvent delay: 3min.
(5) need testing solution preparation: get storax pill for treating coronary heart disease 5g, the accurate title, decide, and puts in the round-bottomed flask, add water 200ml, connect volatile oil determination apparatus, add the water overflow to flask from the analyzer upper end, add ethyl acetate 3ml, connect reflux condensing tube, be heated to little boiling, and kept 3 hours, put coldly, divide and to get acetic acid ethyl fluid, water liquid is used ethyl acetate extraction 2 times again, adds ethyl acetate 5ml at every turn, and combined ethyl acetate liquid is to the 25ml measuring bottle, add ethyl acetate to scale, shake up, as need testing solution.
(6) mix the contrast solution preparation: it is an amount of to take by weighing above-mentioned control medicinal material in storax pill for treating coronary heart disease prescription ratio, and mixing is got 5g, mixes contrast solution with above-mentioned (5) one step preparation method preparation.
(7) under same chromatographic condition, test and record storax pill for treating coronary heart disease test sample chromatogram (see figure 2) and storax pill for treating coronary heart disease mixing contrast color spectrogram (see figure 1) respectively.
(8) whether each chromatographic peak retention time is consistent among comparison diagram 2 and Fig. 1, and then the storax pill for treating coronary heart disease test sample is up-to-standard as if unanimity.
In the present embodiment, respectively the distinguish the flavor of confirmation method of control medicinal material of each chromatographic peak correspondence is as follows in the storax pill for treating coronary heart disease mixing contrast color spectrogram (Fig. 1):
Get borneol, frankincense, santal, elecampane, Soviet Union and fragrant control medicinal material respectively, prepare the control medicinal material solution of respectively distinguishing the flavor of by above-mentioned (5) one step process, and measure, the chromatogram that control medicinal material respectively distinguished the flavor of in record, contrast mixes contrast chromatogram and each flavor control medicinal material chromatogram, mixes 16 chromatographic peaks of contrast chromatogram demonstration, through comparing with each flavor control medicinal material chromatogram, confirm that wherein the 1-6 peak is borneol, 7, the 13-16 peak is frankincense, 9, No. 10 peaks are santal, 11, No. 12 peaks are elecampane, and No. 8 peaks are storax; Each medicinal material of distinguishing the flavor of does not interfere with each other.
The confirmation method of the control medicinal material of respectively distinguishing the flavor of of each chromatographic peak correspondence only need be done once in medicine inspection unit in the above-mentioned storax pill for treating coronary heart disease mixing contrast color spectrogram, can test to the test sample that each pharmaceutical factory provides after the affirmation.
Embodiment 2: utilize high-efficient liquid phase chromatogram technology that each flavour of a drug in the relieving cough, relieving asthma ball are differentiated.
The relieving cough, relieving asthma ball is made up of Chinese ephedra, semen armeniacae amarae, Radix Glycyrrhizae, gypsum four traditional Chinese medicine, has Xin Liangyi to let out, and the effect of clearing lung, relieving asthma is mainly used in cold in the exterior and heat in the interior, and body heat is thirsty, the cough with profuse sputum, and the syndrome characterized by dyspnea circulation of vital energy in the wrong direction, the chest diaphragm is full vexed, the treatment of diseases such as acute bronchitis.Gypsum is mineral drug in this prescription, and no chromatogram behavior so adopt micro-discriminating that it is carried out quality control, adopts high performance liquid chromatography to carry out quality control to three flavor medicines such as other Chinese ephedra, semen armeniacae amarae, Radix Glycyrrhizae.
(1) key instrument
High performance liquid chromatograph (Shimadzu 20A, Japan), balance (Metters AE-163, Switzerland).
(2) material and reagent
Chinese ephedra, semen armeniacae amarae, Radix Glycyrrhizae control medicinal material (middle inspection provides, lot number: 121051-200503,121554-200601,120904-200511)
Test sample relieving cough, relieving asthma ball is available from pharmacy.
Water is pure water, and it is pure that other reagent is analysis.
(3) chromatographic condition: chromatographic column: C
18Post (Shim-pack ODS, 4.6 * 150mm); Phase: A flows: acetonitrile, B:0.01M potassium dihydrogen phosphate (it is 3.5 that triethylamine is transferred pH) carries out gradient elution by subordinate list 1, detects wavelength: 210nm, sample size: 10 μ L, column temperature: 25 ℃.
(4) need testing solution preparation: get the relieving cough, relieving asthma ball, porphyrize is got 1g, accurately claims surely, puts in the tool plug conical flask, and precision adds 0.1% formic acid solution 20ml, and ultrasonic processing 30min is put coldly, shakes up, and filters, and filtrate is as need testing solution.
(5) mix the contrast solution preparation: take by weighing above-mentioned control medicinal material in relieving cough, relieving asthma ball prescription ratio, mixing is got 1g, mixes contrast solution with above-mentioned (4) one step process preparation.
(6) under same chromatographic condition, test and record relieving cough, relieving asthma ball test sample chromatogram (see figure 4) and relieving cough, relieving asthma ball mixing contrast color spectrogram (see figure 3) respectively.
(7) whether each chromatographic peak retention time is consistent among comparison diagram 4 and Fig. 3, if unanimity illustrates that then relieving cough, relieving asthma ball test sample is up-to-standard.
In the present embodiment, respectively the distinguish the flavor of confirmation method of control medicinal material of each chromatographic peak correspondence is identical with embodiment 1 in the relieving cough, relieving asthma ball mixing contrast color spectrogram (Fig. 3).Confirm that the result is: mix the contrast chromatogram and show 6 chromatographic peaks, through and each flavor control medicinal material chromatogram comparison, confirm that wherein the 1-2 peak is Chinese ephedra, 3, the 5-6 peak is Radix Glycyrrhizae, No. 4 peaks are semen armeniacae amarae.Each medicinal material of distinguishing the flavor of does not interfere with each other.
Subordinate list 1: eluent gradient wash-out table
| Time/min | A/％ | B/％ |
| 0～25 | 10～40 | 90～60 |
| 25～28 | 40～10 | 60～90 |
| 28～35 | 10 | 90 |
Claims (2)
1. utilize and mix the method that contrast is differentiated Chinese patent drug, it is characterized in that concrete steps are as follows:
(1) obtain the test sample chromatogram:
A: take by weighing test sample;
B: preparation need testing solution;
The extracting method of selecting to adapt according to the character of the contained chemical constitution of crude drug of respectively distinguishing the flavor of in the described test sample prepares need testing solution;
C: select the chromatographic condition that adapts according to the character of the contained chemical analysis of crude drug of respectively distinguishing the flavor of in the described test sample, test is record test sample chromatogram also;
(2) obtain mixing contrast color spectrogram:
Described mixing contrast refers to get the product of control medicinal material in prescription ratio mixing gained of respectively distinguishing the flavor of in the described test sample;
A: take by weighing and mix contrast with described test sample equivalent described;
B: preparation mixes contrast solution: the preparation of preparation method and process conditions and described need testing solution is identical;
C: under the same chromatographic condition in going on foot with above-mentioned (1), test and record described mixing contrast color spectrogram;
(3) whether each chromatographic peak retention time is consistent in contrast test sample chromatogram and the mixing contrast color spectrogram.
2. utilization according to claim 1 mixes the method that contrast is differentiated Chinese patent drug, it is characterized in that the instrument that the test color spectrogram adopts comprises high performance liquid chromatograph, gas chromatograph, Ultra Performance Liquid Chromatography instrument and liquid chromatography mass combined instrument, gas chromatograph-mass spectrometer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010221934 CN101936974B (en) | 2010-07-09 | 2010-07-09 | Method for identifying Chinese patent drugs by using mixed contrast |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010221934 CN101936974B (en) | 2010-07-09 | 2010-07-09 | Method for identifying Chinese patent drugs by using mixed contrast |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101936974A CN101936974A (en) | 2011-01-05 |
| CN101936974B true CN101936974B (en) | 2013-09-04 |
Family
ID=43390413
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010221934 Expired - Fee Related CN101936974B (en) | 2010-07-09 | 2010-07-09 | Method for identifying Chinese patent drugs by using mixed contrast |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101936974B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103018391B (en) * | 2011-09-23 | 2015-03-11 | 四川科伦药物研究有限公司 | Quality control method of Spica Prunellae, mulberry leaf and chrysanthemum granules |
| CN108152427A (en) * | 2018-02-13 | 2018-06-12 | 南京市食品药品监督检验院 | A kind of Chinese patent drug method for quick identification based on LC-MS |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1470876A (en) * | 2002-07-25 | 2004-01-28 | 浙江大学 | Chinese medicine quality control and evaluation method |
-
2010
- 2010-07-09 CN CN 201010221934 patent/CN101936974B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1470876A (en) * | 2002-07-25 | 2004-01-28 | 浙江大学 | Chinese medicine quality control and evaluation method |
Non-Patent Citations (4)
| Title |
|---|
| 孔铭等.月月舒饮片汤剂与其免煎配方的指纹图谱比较.《中国实验方剂学杂志》.2007,第13卷(第3期),5-6. |
| 月月舒饮片汤剂与其免煎配方的指纹图谱比较;孔铭等;《中国实验方剂学杂志》;20070331;第13卷(第3期);5-6 * |
| 金文姗.高效液相色谱比较黄栀胶囊全方合煎何分煎混合对成分的影响.《中药研究与信息》.2002,第4卷(第1期),20-21. |
| 高效液相色谱比较黄栀胶囊全方合煎何分煎混合对成分的影响;金文姗;《中药研究与信息》;20020131;第4卷(第1期);20-21 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101936974A (en) | 2011-01-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104459003B (en) | The construction method of contracting spring standard preparation finger-print and characteristic spectrum and quality determining method | |
| CN101991661B (en) | Method for detecting Chinese patent drug containing at least two of white paeony root, ginseng, salvia miltiorrhiza, sweet wormwood, liquorice and angelica sinensis | |
| CN105806975A (en) | Method for establishing lonicerae and forsythiae powder UPLC fingerprint spectrum | |
| CN105477166A (en) | Preparation method of pubescent angelica and mistletoe decoction formula granules and quality control method thereof | |
| WO2022022065A1 (en) | Method for establishing fingerprint spectrum of cervicodynia treatment granules, and application thereof | |
| CN105301168B (en) | The detection method of dredging collateral resolving sputum capsule | |
| CN102426205B (en) | Detection method of thrombus sumalin capsules | |
| CN114689780A (en) | Multi-component quality detection method for Baoyin decoction extract | |
| CN107402265B (en) | Detection method of Kangyun granule fingerprint | |
| CN101744946B (en) | Chinese medicinal composition and detection method for Chinese medicinal composition preparation | |
| CN101936974B (en) | Method for identifying Chinese patent drugs by using mixed contrast | |
| CN100446805C (en) | Medicine for treating chronic diarrhoea | |
| CN105004833A (en) | Detection method for traditional Chinese medicine preparation for treating acute gouty arthritis and gout | |
| CN104101657B (en) | Method for determining content of multiple components in Chinese medicinal composition preparation | |
| CN105548411B (en) | In a kind of ZHENGTIAN WAN preparation in the construction method and ZHENGTIAN WAN preparation of the characteristic spectrum of volatile ingredient volatile ingredient detection method | |
| CN108226325A (en) | Roripa montana gives birth to the method for building up of arteries and veins oral liquid composition finger-print | |
| CN101884746A (en) | Method for detecting capsules for treating cough with asthma | |
| CN104922587A (en) | Preparation method of swelling-removing and pain-relieving paste and quality-detecting method of swelling-removing and pain-relieving paste | |
| CN104277086A (en) | Extraction method of scutellarin in scutellariae barbatae | |
| CN112881540A (en) | Method for detecting bupleurum chinense and vinegar bupleurum chinense formula granules | |
| CN114910576B (en) | Method for detecting aconite monoester type alkaloid component in cassia twig, chinese herbaceous peony and rhizoma anemarrhenae soup | |
| CN102049028A (en) | Method for establishing HPLC (high performance liquid chromatography) fingerprint graphic for ointment for unblocking collaterals and relieving pain as well as standard fingerprint graphic thereof | |
| CN114689776B (en) | Construction method of high-efficiency liquid-phase characteristic spectrum of lindera root decoction | |
| CN106596777B (en) | The method of quality control of Dandengtongnao preparation | |
| CN114848693A (en) | Wine-washed angelica sinensis decoction pieces and processing method, quality detection method and application thereof |
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 | ||
| 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: 20130904 Termination date: 20190709 |