CN100392396C - Method for checking Cinnamomum cassia medicinal material by using traditional medicine fingerprint pattern technology - Google Patents
Method for checking Cinnamomum cassia medicinal material by using traditional medicine fingerprint pattern technology Download PDFInfo
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- CN100392396C CN100392396C CNB2005101205762A CN200510120576A CN100392396C CN 100392396 C CN100392396 C CN 100392396C CN B2005101205762 A CNB2005101205762 A CN B2005101205762A CN 200510120576 A CN200510120576 A CN 200510120576A CN 100392396 C CN100392396 C CN 100392396C
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Abstract
The invention discloses a method for detecting the cinnamon 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 cinnamon medicinal materials are built; the second step, the common mode graph spectrums of the fingerprint graph spectrum of cinnamon 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 cinnamon 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 cinnamon medicinal materials.
Description
(1) technical field:
The invention belongs to a kind of detection method of Chinese crude drug, specifically is the method with traditional Chinese medicine fingerprint technology for detection Chinese cassia tree medicinal material.
(2) background technology:
" 2000 editions Chinese cassia trees of recording of Chinese pharmacopoeia are the dry bark of canella Chinese cassia tree Cinnamomum cassia Presl, main product in Guangxi, Guangdong Er Sheng.Contain volatile oil in the Chinese cassia tree, principal ingredient is a cinnaldehydrum in the oil, accounts for about 85%; Also contain chemical constitutions such as terpene, catechin, epicatechin class, polyhydric phenol and tannin.At present, Chinese Pharmacopoeia only adopts thin-layered chromatography that it is carried out qualitative analysis to the detection of Chinese cassia tree, therefore, and the overall picture of reaction Chinese cassia tree medicinal material that can not be complete.The fingerprint map analyzing technology can quantize to detect the macroscopic quality information of Chinese crude drug effectively, it is compared with existing single index components or active component detection, its contained information is comprehensive multi-level and concrete the quantification, therefore science and rationally more, the pharmacology that also more meets Chinese medicine, the final examination criteria of traditional Chinese medicine quality is also safer and effective.
(3) summary of the invention:
Purpose of the present invention is exactly to propose a kind of method with traditional Chinese medicine fingerprint technology for detection Chinese cassia tree medicinal material.
This method comprises the steps:
The first step is set up Chinese cassia tree medicinal material reference fingerprint
1. the preparation of standard solution
It is an amount of to get the cinnaldehydrum standard items, adds the solution that methyl alcohol is made every 1mg/ml, promptly;
2. the preparation of reference substance solution
The powder 5.0g that learns from else's experience and be accredited as the Chinese cassia tree medicinal material puts in the tool plug conical flask, adds 70% methyl alcohol 35ml, and jolting is fully soaked into it, soaks under the room temperature after 24 hours, filters, and the accurate above-mentioned solution of 1ml of drawing is put in the 10ml headspace sampling bottle, seals, promptly;
Chromatographic condition
Chromatographic column Agilent HP-5,30m * 320 μ m * 0.25 μ m
Injector temperature: 230 ℃
Fid detector temperature: 260 ℃
Heating schedule: initial 100 ℃, keep 1min, 4.5 ℃/min rises to 180 ℃, keeps 1min, and 10 ℃/min rises to 220 ℃, keeps 10min;
Carrier gas is N2, flow velocity 1.5ml/min, and current constant mode is not shunted;
Injector: G1888A head space automatic sampler, 90 ℃ of head space bottle temperature, 105 ℃ of sampling valve temperature, 120 ℃ of transmission line temperature, head space bottle equilibration time 15min, head space bottle pressurising time 0.2min, quantitatively ring filling time 0.2min quantitatively encircles equilibration time 0.5min, sample injection time 1min;
3. chromatograph Agilent6890
It is pure that top grade is produced in reagent methyl alcohol Tianjin
Water pure water second distillation
The nitrogen high pure nitrogen, purity 99.999%
4. detect
Above-mentioned reference substance solution and standard solution are respectively through the head-space sampler sample introduction, and gas chromatograph for determination promptly gets reference substance and standard items gas chromatogram.
In the described Chinese cassia tree medicinal material reference fingerprint, have 5 characteristic peaks, wherein No. 2 peaks are cinnaldehydrum, and are consistent with the standard items finger-print.The foundation of Chinese cassia tree medicinal material reference fingerprint makes the quality control of product that standard very clear and definite, directly perceived, easy operating arranged, and only needs during use testing result is compared with it and can reach a conclusion.
In second step, set up Chinese cassia tree medicinal materials fingerprint common pattern collection of illustrative plates
Collected and 10 batch samples through being accredited as the Chinese cassia tree 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 Chinese cassia tree medicinal material and standard items finger-print respectively; The auxiliary similarity evaluation system of machine calculates as calculated, can draw Chinese cassia tree medicinal material common pattern collection of illustrative plates;
The effect one of setting up the common pattern collection of illustrative plates is can be with the Chinese cassia tree medicinal materials fingerprint input COMPUTER CALCULATION test sample of gained and the related coefficient between the total mode chart spectrum, investigate the similarity between test sample and the total mode chart spectrum theoretically, thereby make more objective science of controllable quality; The 2nd, can make things convenient under the different places of production, different cultivars, the different ecological environment to compare between each kind, 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 Chinese cassia tree 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 5 characteristic peaks identical with reference fingerprint in the chromatogram, wherein No. 2 peaks are cinnaldehydrum, should be consistent with the standard items finger-print;
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;
Principle of the present invention is based on the volatile ingredient that mainly contains in the Chinese cassia tree medicinal material, therefore, adopts the vapor-phase chromatography relatively sensitiveer to volatile ingredient, and the group detects to material, 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 Chinese cassia tree 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 Chinese cassia tree medicinal materials fingerprint common pattern collection of illustrative plates, and the related coefficient between definite test sample finger-print and the corresponding common pattern collection of illustrative plates is 0.9000; Therefore, utilize this method to detect to the Chinese cassia tree medicinal material.
(4) description of drawings:
Fig. 1 is a Chinese cassia tree medicinal material reference fingerprint;
Fig. 2 is a Chinese cassia tree medicinal materials fingerprint common pattern collection of illustrative plates;
Fig. 3 is cinnaldehydrum standard items finger-prints;
Fig. 4 is the finger-print similarity evaluation figure as a result that is numbered 20041008,20041227,20050228,20050329,20050516 Chinese cassia tree medicinal materials.
(5) embodiment:
The detection of embodiment 1 Chinese cassia tree medicinal material
1, crude drug source Guangdong
2, sample number into spectrum 20041008
3, the preparation of need testing solution
Prepare Chinese cassia tree medicinal material 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 5 characteristic peaks identical with Chinese cassia tree medicinal material reference fingerprint in the chromatogram, wherein No. 2 peaks are cinnaldehydrum, and are consistent with the standard items finger-print; Test sample finger-print and Chinese cassia tree medicinal materials fingerprint common pattern the collection of illustrative plates auxiliary similarity evaluation system of machine as calculated calculate, and related coefficient is 0.9950, greater than 0.9000; Therefore, can judge that this test sample meets the quality standard about the Chinese cassia tree medicinal material of our company's revision.
The detection of embodiment 2 Chinese cassia tree medicinal materials
1, crude drug source Guangxi
2, sample number into spectrum 20041227
3, the preparation of need testing solution
Prepare Chinese cassia tree medicinal material 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 5 characteristic peaks identical with Chinese cassia tree medicinal material reference fingerprint in the chromatogram, wherein No. 2 peaks are cinnaldehydrum, and are consistent with the standard items finger-print; Test sample finger-print and Chinese cassia tree medicinal materials fingerprint common pattern the collection of illustrative plates auxiliary similarity evaluation system of machine as calculated calculate, and related coefficient is 0.9887, greater than 0.9000; Therefore, can judge that this test sample meets the quality standard about the Chinese cassia tree medicinal material of our company's revision.
The detection of embodiment 3 Chinese cassia tree medicinal materials
1, crude drug source Guangdong
7, sample number into spectrum 20050228
8, the preparation of need testing solution
Prepare Chinese cassia tree medicinal material need testing solution with above-mentioned same procedure;
9, with above-mentioned same procedure preparation standard product solution;
10, measure standard items and need testing solution to be measured with above-mentioned same procedure;
11, the result judges
Detected 5 characteristic peaks identical with Chinese cassia tree medicinal material reference fingerprint in the chromatogram, wherein No. 2 peaks are cinnaldehydrum, and are consistent with the standard items finger-print; Test sample finger-print and Chinese cassia tree medicinal materials fingerprint common pattern the collection of illustrative plates auxiliary similarity evaluation system of machine as calculated calculate, and related coefficient is 0.9912, greater than 0.9000; Therefore, can judge that this test sample meets the quality standard about the Chinese cassia tree medicinal material of our company's revision.
Claims (2)
1. with the method for traditional Chinese medicine fingerprint technology for detection Chinese cassia tree medicinal material, comprise the steps:
The first step is set up Chinese cassia tree medicinal material reference fingerprint
1. the preparation of standard solution
It is an amount of to get the cinnaldehydrum standard items, adds the solution that methyl alcohol is made 1mg/ml, promptly;
2. the preparation of reference substance solution
The powder 5.0g that learns from else's experience and be accredited as the Chinese cassia tree medicinal material puts in the tool plug conical flask, adds 70% methyl alcohol 35ml, and jolting is fully soaked into it, soaks under the room temperature after 24 hours, filters, and the accurate above-mentioned solution of 1ml of drawing is put in the 10ml headspace sampling bottle, seals, promptly;
3. chromatographic condition
Chromatographic column Agilent HP-5,30m * 320 μ m * 0.25 μ m
Injector temperature: 230 ℃
Fid detector temperature: 260 ℃
Heating schedule: initial 100 ℃, keep 1min, 4.5 ℃/min rises to 180 ℃, keeps 1min, and 10 ℃/min rises to 220 ℃, keeps 10min;
Carrier gas is N2, flow velocity 1.5ml/min, and current constant mode is not shunted;
Injector: G1888A head space automatic sampler, 90 ℃ of head space bottle temperature, 105 ℃ of sampling valve temperature, 120 ℃ of transmission line temperature, head space bottle equilibration time 15min, head space bottle pressurising time 0.2min, quantitatively ring filling time 0.2min quantitatively encircles equilibration time 0.5min, sample injection time 1min;
4. detect
Above-mentioned reference substance solution and standard solution are respectively through the head-space sampler sample introduction, and gas chromatograph for determination promptly gets reference substance and standard items gas chromatogram;
In second step, set up Chinese cassia tree medicinal materials fingerprint common pattern collection of illustrative plates
Collected and 10 batch samples through being accredited as the Chinese cassia tree 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 Chinese cassia tree medicinal material and standard items finger-print respectively; The auxiliary similarity evaluation system of machine calculates as calculated, can draw Chinese cassia tree medicinal material common pattern collection of illustrative plates;
In the 3rd step, test sample detects
1. the preparation of need testing solution
Prepare Chinese cassia tree 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 5 characteristic peaks identical with reference fingerprint in the chromatogram, wherein No. 2 peaks are cinnaldehydrum, should be consistent with the standard items finger-print;
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 traditional Chinese medicine fingerprint technology for detection Chinese cassia tree medicinal material 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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| CNB2005101205762A CN100392396C (en) | 2005-12-28 | 2005-12-28 | Method for checking Cinnamomum cassia medicinal material by using traditional medicine fingerprint pattern technology |
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| CN100392396C true CN100392396C (en) | 2008-06-04 |
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| CN101975845A (en) * | 2010-09-21 | 2011-02-16 | 成都中医药大学 | Automatic detecting system for quality of traditional Chinese medicines |
| CN107167544B (en) * | 2016-03-07 | 2019-02-12 | 亚宝药业集团股份有限公司 | A method for determining active ingredients in a medicinal composition for invigorating the spleen, warming the middle, dispelling cold and relieving diarrhea and establishing a fingerprint |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6569468B2 (en) * | 2000-09-13 | 2003-05-27 | Jiangsu Kanion Pharmaceutical Co., Ltd. | Cinnamomi and poria composition, method to prepare same and uses thereof |
| CN1670523A (en) * | 2004-03-16 | 2005-09-21 | 金陵药业股份有限公司 | Method for quality control of injections for treating thromboangitis diseases |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6569468B2 (en) * | 2000-09-13 | 2003-05-27 | Jiangsu Kanion Pharmaceutical Co., Ltd. | Cinnamomi and poria composition, method to prepare same and uses thereof |
| CN1670523A (en) * | 2004-03-16 | 2005-09-21 | 金陵药业股份有限公司 | Method for quality control of injections for treating thromboangitis diseases |
Non-Patent Citations (2)
| Title |
|---|
| 肉桂及其混伪品的HSGC-MS的实验比较研究. 张海霞等.中草药，第34卷第1期. 2003 |
| 肉桂及其混伪品的HSGC-MS的实验比较研究. 张海霞等.中草药，第34卷第1期. 2003 * |
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