CN100392398C - Method for identifying Korea barren wort medicinal material by using traditional medicine fingerprint pattern technology - Google Patents
Method for identifying Korea barren wort medicinal material by using traditional medicine fingerprint pattern technology Download PDFInfo
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- CN100392398C CN100392398C CNB2005101205781A CN200510120578A CN100392398C CN 100392398 C CN100392398 C CN 100392398C CN B2005101205781 A CNB2005101205781 A CN B2005101205781A CN 200510120578 A CN200510120578 A CN 200510120578A CN 100392398 C CN100392398 C CN 100392398C
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Abstract
The invention discloses a method for detecting the Korea barrenwort medicinal materials by the traditional Chinese drug fingerprint graph spectrum technique, the method includes following steps: the first step, the comparison fingerprint graph spectrums of Korea barrenwort medicinal materials are built; the second step, the common mode graph spectrums of the fingerprint graph spectrum of Korea barrenwort medicinal materials are built; the third step, detect the sample; and the graph spectrum of sample is compared with the comparison fingerprint graph spectrums, and the estimating system of auxiliary similarity is input the computer and calculate the similarity to obtain the correlation coefficient and can make a detection solution; the characteristics of the method are those: (1) it can represent the quality of Korea barrenwort medicinal materials macroscopically; (2) it is definitude and intuitionistic, and has good exclusive property, characteristic property, repeatability and operation; (3) it can be used to identify the true or false of the Korea barrenwort medicinal materials.
Description
(1) technical field:
The invention belongs to a kind of discrimination method of Chinese crude drug, specifically is the method for differentiating korean epimedium herb with the traditional Chinese medicine fingerprint technology.
(2) background technology:
" 2000 editions barrenwort that record of Chinese pharmacopoeia are the dry aerial parts of Berberidaceae plant barrenwort Epimedium brevicornum Maxim, arrow leaf barrenwort Epimediumsagittatum (Sieb.et Zucc.) Maxim, pubescence barrenwort Epimediumpubescens Maxim, Wushan barrenwort Epimedium wushanense T.S.Ying or korean epimedium herb Epimedium koreanum Nakai.Owing to be subjected to the influence of factors such as kind, weather, the place of production and ecologic environment, the contained flavones ingredient of epimedium herbs not of the same race, the different places of production is widely different, therefore, at present only carry out qualitative, quantitative test, facts have proved and effectively to control its product quality at certain effective constituent or the index of certain medicinal material.And the traditional Chinese medicine fingerprint technology has been used for reference in " general character " feature of seeking " only " exactly and has been compared principle, with Chinese medicine material medicinal material, medicine materical crude slice, semi-manufacture, finished product etc. after suitably handling, adopt certain analysis means, obtain to indicate the collection of illustrative plates at the total peak of its characteristic, so as to homogeneity and the stability of telling truth from falsehood, estimate raw medicinal material, semi-manufacture and end product quality.Therefore, this technology is applied in the discriminating of Chinese crude drug to the differentiation medicinal material place of production, fixedly raw material sources, improve and stabilized product quality has crucial meaning.
(3) summary of the invention:
Purpose of the present invention is exactly to propose a kind of method of differentiating Korea barren wort medicinal material with the traditional Chinese medicine fingerprint technology.
This method comprises the steps:
The first step is set up the Korea barren wort medicinal material reference fingerprint
1. the preparation of standard solution
It is an amount of to get the icariin standard items, makes the solution of every 1mg/ml with 70% methyl alcohol, promptly;
2. the preparation of reference substance solution
The powder 1.0g that learns from else's experience and be accredited as Korea barren wort medicinal material puts in the tool plug conical flask, the accurate 70% methyl alcohol 10ml that adds, and ultrasonic Extraction 30min filters, and filtrate is filtered with 0.45 μ m miillpore filter is smart, promptly;
3. chromatographic condition
Chromatographic column Hypersil C18 post 4.6 * 250mm, 5 μ m, theoretical cam curve should be not less than 3000 by icariin;
The moving phase acetonitrile-water is the eluent gradient wash-out, and when retention time was 0min, 5min, 60min, 75min, the volume ratio of acetonitrile and water was respectively 2: 98,2: 98, and 40: 60,40: 60;
Flow velocity: 1.0ml/ minute
Detect wavelength: 272nm
Column temperature: 30 ℃
4. key instrument and reagent
Chromatograph Varian Associates, Inc. (US) 611 Hansen Way, Palo Alto, California 94303, U.S.A. instrument (230 pumps, 330 detecting device 7725i manual injector AT-830 column ovens)
It is pure that top grade is produced in reagent methyl alcohol Tianjin
It is pure that analysis is produced in isoamylol Tianjin
Acetonitrile USAJ.T.Baker chromatographically pure
Water Robust pure water single flash
Korea barren wort medicinal material sample Liaoning Heng Ren
5. detect
Precision is drawn reference substance solution and each 10 μ l injection liquid chromatograph of standard solution respectively, according to " 2000 editions appendix high effective liquid chromatography for measuring of Chinese pharmacopoeia get Korea barren wort medicinal material reference fingerprint and standard items finger-print;
In the described Korea barren wort medicinal material reference fingerprint, have 19 characteristic peaks, wherein No. 13 peaks are excessive foreign sheep leaves of pulse plants glycosides, and consistent with the standard items finger-print, 10～No. 14 the peak is the five fingers shape, and No. 18 is one group of weak absorption;
Towards the foundation of the bright epimedium herb reference fingerprint in danger, make the quality control of product that standard very clear and definite, directly perceived, easy operating arranged, only need during use testing result is compared with it and can reach a conclusion.
In second step, set up Korea barren wort medicinal material finger-print common pattern collection of illustrative plates
Collected and 10 batch samples through being accredited as Korea barren wort medicinal material are prepared need testing solution by the preparation method of reference substance solution, by above-mentioned standard solution preparation method preparation standard product solution, and detect by above-mentioned same procedure one by one, obtain corresponding finger-print of each batch Korea barren wort medicinal material and standard items finger-print respectively; The auxiliary similarity evaluation system of machine calculates as calculated, can draw the common pattern collection of illustrative plates of Korea barren wort medicinal material finger-print;
The effect one of setting up the common pattern collection of illustrative plates is can be with the related coefficient between Korea barren wort medicinal material testing result input COMPUTER CALCULATION test sample and the total mode chart spectrum, investigate the similarity between test sample and the total mode chart spectrum theoretically, thereby make the discrimination standard of quality more objective, science more; The 2nd, carry out differentiation relatively between each kind under the convenient different places of production, different cultivars, the different ecological environment, to investigate the homogeneity and the stability of product, guarantee to provide the product of high-quality for the consumer.
In the 3rd step, test sample detects
1. the preparation of need testing solution
Prepare the Korea barren wort medicinal material need testing solution with above-mentioned same procedure;
2. with above-mentioned same procedure preparation standard product solution;
3. measure standard items and test sample to be measured with above-mentioned same procedure;
4. interpretation of result is judged
Should detect 19 (group) characteristic peaks identical with reference fingerprint in the chromatogram, wherein No. 13 peaks are icariin, should be consistent with the standard items finger-print; 10～No. 14 the peak is the five fingers shape, and No. 18 is one group of weak absorption;
With test sample finger-print and corresponding common pattern collection of illustrative plates as calculated the auxiliary similarity evaluation system of machine calculate, related coefficient should be greater than 0.9000;
Principle of the present invention is based on and mainly contains the flavonoid glycoside composition in the Korea barren wort medicinal material, comprise icariine A, Da Hua icariin C, epimidin B, epimidin C, icariin etc., because its composition has strong absorption in the ultraviolet region, therefore, adopt ultraviolet method that its Flavonoid substances group is detected, on the whole, product quality is controlled on the macroscopic view; In research process, also respectively extracting method, detection method, chromatographic condition and system flexibility are investigated, satisfy requirements such as accuracy, stability, reappearance simultaneously, with gathered and through the sample of expert appraisal product in contrast, the finger-print that it drew is as the Korea barren wort medicinal material reference fingerprint; The computer aided similarity evaluation system of recommending through pharmacopoeia commission according to the finger-print of gather 10 batch samples by the modernization of cmm center exploitation of Hunan Central South University calculates, set up the common pattern collection of illustrative plates of Korea barren wort medicinal material finger-print, and the corresponding coefficient between definite test sample finger-print and the corresponding common pattern collection of illustrative plates is 0.9000; Therefore, utilize this method to differentiate to Korea barren wort medicinal material.
(4) description of drawings:
Fig. 1 is the Korea barren wort medicinal material reference fingerprint;
Fig. 2 is the total common pattern collection of illustrative plates of Korea barren wort medicinal material finger-print;
Fig. 3 is icariin standard items finger-prints;
Fig. 4 is the finger-print similarity evaluation figure as a result that is numbered 20,040,816 20,041,007 20041203 epimedium herbs;
Fig. 5 is numbered 2004-4-8 epimedium herb finger-print.
(5) embodiment:
The discriminating of embodiment 1 epimedium herb
1, crude drug source Liaoning Heng Ren
2, sample number into spectrum 20040816
3, the preparation of need testing solution
Prepare the epimedium herb need testing solution with above-mentioned same procedure;
4, with above-mentioned same procedure preparation standard product solution;
5, measure standard items and need testing solution to be measured with above-mentioned same procedure;
6, the result judges
Detected 19 (group) characteristic peaks identical with the Korea barren wort medicinal material reference fingerprint in the chromatogram, wherein No. 13 peaks are icariin, and are consistent with the standard items finger-print; 10～No. 14 the peak is the five fingers shape, and No. 18 is one group of weak absorption; Test sample finger-print and Korea barren wort medicinal material finger-print common pattern the collection of illustrative plates auxiliary similarity evaluation system of machine as calculated calculate, and related coefficient is 0.9529, greater than 0.9000; Therefore, can judge that this test sample is a korean epimedium herb.
The discriminating of embodiment 2 epimedium herbs
1, crude drug source Liaoning Heng Ren
2, sample number into spectrum 20041007
3, the preparation of need testing solution
Prepare the epimedium herb need testing solution with above-mentioned same procedure;
4, with above-mentioned same procedure preparation standard product solution;
5, measure standard items and need testing solution to be measured with above-mentioned same procedure;
6, the result judges
Detected 19 (group) characteristic peaks identical with the Korea barren wort medicinal material reference fingerprint in the chromatogram, wherein No. 13 peaks are icariin, and are consistent with the standard items finger-print; 10～No. 14 the peak is the five fingers shape, and No. 18 is one group of weak absorption; Test sample finger-print and Korea barren wort medicinal material finger-print common pattern the collection of illustrative plates auxiliary similarity evaluation system of machine as calculated calculate, and related coefficient is 0.9547, greater than 0.9000; Therefore, can judge that this test sample is a korean epimedium herb.
The discriminating of embodiment 3 epimedium herbs
1, crude drug source Liaoning Heng Ren
2, sample number into spectrum 20041203
3, the preparation of need testing solution
Prepare the epimedium herb need testing solution with above-mentioned same procedure;
4, with above-mentioned same procedure preparation standard product solution;
5, measure standard items and need testing solution to be measured with above-mentioned same procedure;
6, the result judges
Detected 19 (group) characteristic peaks identical with the Korea barren wort medicinal material reference fingerprint in the chromatogram, wherein No. 13 peaks are icariin, and are consistent with the standard items finger-print; 10～No. 14 the peak is the five fingers shape, and No. 18 is one group of weak absorption; Test sample finger-print and Korea barren wort medicinal material finger-print common pattern the collection of illustrative plates auxiliary similarity evaluation system of machine as calculated calculate, and related coefficient is 0.9737, greater than 0.9000; Therefore, can judge that this test sample is the excessive foreign sheep leaves of pulse plants of Korea.
The discriminating of embodiment 4 epimedium herbs
1, Yuanling, crude drug source Hunan
2, sample number into spectrum 2004-4-8
3, the preparation of need testing solution
Prepare the epimedium herb need testing solution with above-mentioned same procedure;
4, with above-mentioned same procedure preparation standard product solution;
5, measure standard items and need testing solution to be measured with above-mentioned same procedure;
6, the result judges
Gained test sample finger-print and Korea barren wort medicinal material reference fingerprint differ bigger, lack at " Five Fingers Peak " that Korea barren wort medicinal material had of retention time about 50 minutes; And test sample finger-print and Korea barren wort medicinal material finger-print common pattern the collection of illustrative plates auxiliary similarity evaluation system of machine as calculated calculate, and related coefficient is 0.4430 only, less than 0.9000; Can judge that this test sample is not a korean epimedium herb.
Claims (2)
1. differentiate the method for Korea barren wort medicinal material with the traditional Chinese medicine fingerprint technology, may further comprise the steps:
The first step is set up the Korea barren wort medicinal material reference fingerprint
1. the preparation of standard solution
It is an amount of to get the icariin standard items, makes the solution of 1mg/ml with 70% methyl alcohol, promptly;
2. the preparation of reference substance solution
The powder 1.0g that learns from else's experience and be accredited as Korea barren wort medicinal material puts in the tool plug conical flask, the accurate 70% methyl alcohol 10ml that adds, and ultrasonic Extraction 30min filters, and filtrate is filtered with 0.45 μ m miillpore filter is smart, promptly;
3. chromatographic condition
Chromatographic column Hypersil C18 post 4.6 * 250mm, 5 μ m, theoretical cam curve should be not less than 3000 by icariin;
The moving phase acetonitrile-water is the eluent gradient wash-out, and when retention time was 0min, 5min, 60min, 75min, the volume ratio of acetonitrile and water was respectively 2: 98,2: 98, and 40: 60,40: 60;
Flow velocity: 1.0ml/ minute
Detect wavelength: 272nm
Column temperature: 30 ℃
4. detect
Precision is drawn reference substance solution and each 10 μ l injection liquid chromatograph of standard solution respectively, according to high effective liquid chromatography for measuring, gets Korea barren wort medicinal material reference fingerprint and standard items finger-print;
In second step, set up Korea barren wort medicinal material finger-print common pattern collection of illustrative plates
Collected and 10 batch samples through being accredited as Korea barren wort medicinal material are prepared need testing solution by the preparation method of reference substance solution, by above-mentioned standard solution preparation method preparation standard product solution, and detect by above-mentioned same procedure one by one, obtain corresponding finger-print of each batch Korea barren wort medicinal material and standard items finger-print respectively; The auxiliary similarity evaluation system of machine calculates as calculated, can draw the common pattern collection of illustrative plates of Korea barren wort medicinal material finger-print;
In the 3rd step, test sample detects
1. the preparation of need testing solution
Prepare the Korea barren wort medicinal material need testing solution respectively with above-mentioned same procedure;
2. with above-mentioned same procedure difference preparation standard product solution;
3. measure standard items and test sample to be measured with above-mentioned same procedure;
4. interpretation of result is judged
Should detect the 19/stack features peak identical with reference fingerprint in the chromatogram, wherein No. 13 peaks are icariin, should be consistent with the standard items finger-print; 10～No. 14 the peak is the five fingers shape, and No. 18 is one group of weak absorption;
Test sample finger-print and corresponding common pattern the collection of illustrative plates auxiliary similarity evaluation system of machine as calculated calculate, and related coefficient should be greater than 0.9000.
2. the method with fingerprint pattern technology discriminating korean epimedium herb according to claim 1 is characterized in that: described computer aided similarity evaluation system is by being developed by Hunan Central South University modernization of cmm center that pharmacopoeia commission is recommended.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104749306B (en) * | 2013-12-30 | 2016-06-22 | 广州白云山陈李济药厂有限公司 | A kind of method of the finger printing building Herba Epimedii extract |
| CN104820049B (en) * | 2015-03-17 | 2016-06-08 | 中山市中智药业集团有限公司 | The finger printing common pattern of Herba Epimedii breaking cellular wall decoction pieces builds and quality determining method |
| CN107655994B (en) * | 2017-09-30 | 2020-07-03 | 天津中医药大学 | Method for measuring content of 16 chemical components in epimedium extract |
| CN110672747A (en) * | 2019-10-23 | 2020-01-10 | 劲牌生物医药有限公司 | Method for detecting epimedium component, method for identifying variety of epimedium and application |
| CN113495102B (en) * | 2020-04-03 | 2022-10-25 | 国药集团同济堂（贵州）制药有限公司 | Method for identifying epimedium based on UPLC-Q-TOF-MS technology |
| CN113834879B (en) * | 2020-06-23 | 2023-10-20 | 国药集团同济堂（贵州）制药有限公司 | Establishment and application of epimedium flavone component fingerprint based on SPE technology |
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| JPH04159295A (en) * | 1990-10-24 | 1992-06-02 | Tsumura & Co | Flavonoid glucoside and 5-lipoxygenase inhibitor containing the flavonoid as active ingredient |
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