CN1425909A - Infrared spectrum detection method for effective component in traditional Chinese medicine drip pills preparation - Google Patents
Infrared spectrum detection method for effective component in traditional Chinese medicine drip pills preparation Download PDFInfo
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- CN1425909A CN1425909A CN 02159972 CN02159972A CN1425909A CN 1425909 A CN1425909 A CN 1425909A CN 02159972 CN02159972 CN 02159972 CN 02159972 A CN02159972 A CN 02159972A CN 1425909 A CN1425909 A CN 1425909A
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Abstract
The infrared spectrum detection method for effective component in traditional Chinese medicine drip pills preparation includes the following steps: measuring the infrared spectrum of any known component in Chinese medicine drip pills; pre-treatment of the infrared spectrum of the said component and establishing the quantitative relation between the absorption photometric amount and content of the component and quantitative mathematic model; and test the infrared spectrum of the component in unknown content and calculating the content by means of the mathematic model. The said method can perform in-line test for detecting and regulating content at will, and this is favorable to raising product quality.
Description
Technical field
The present invention relates to a kind of infrared spectrum detection method of traditional Chinese medicine ingredients, particularly to the infrared spectrum detection method of effective constituent in the Chinese medicine dropping pill formulation.
Background technology
Infrared spectrum is as " molecular fingerprint ", can utilize the frequency of characteristic absorption peak, infer in the molecule and have a certain group or key, and then again by the displacement of characteristic absorption peak frequency, deduction is in abutting connection with group or key, determine the chemical constitution of molecule and, can carry out qualitative and quantitative analysis its potpourri and compound by the change of characteristic absorption peak intensity.The infrared spectrum detection technique with its detected object extensively, can realize that advantages such as non-destructive detects, specimen preparation is simple, detection speed is fast are applied to a lot of fields.The infrared spectrum detection method is used in the field of Chinese medicines its special advantages, the evaluation method of at first this science can be avoided the artificial property that experience among the people identifies and the complicacy of conventional authentication method, accelerate the process of modernization of cmm, help making Chinese herbal product to enter the international market as early as possible; Next infrared spectrum detection method, specimen preparation is simple, and analysis speed is fast, and expense is lower, applied range.
The infrared spectrum detection technique mainly is the discriminating of Chinese crude drug and the foundation of traditional Chinese medicine fingerprint in the application of the field of Chinese medicines at present.Publication number is that the infrared spectrum detection method of the CN1274841A patented claim certified products root bark of white mulberry is exactly an example that adopts infrared spectrum technology to differentiate the certified products root bark of white mulberry.This patent with the Chinese medicine crude drug certified products root bark of white mulberry and equal, belong to together or equal, do not belong to the adulterant kind together and make a distinction from objectively responding of molecular structure, employing be transmission beam method in the infrared spectrum.With the relative transmittance value of sample characteristic absorption peak transmissivity whether less than 1 and characteristic absorption peak whether be the unimodal certified products root bark of white mulberry that takes a decision as to whether.Traditional Chinese medicine fingerprint (comprising Chinese medicine material, Chinese medical extract and Chinese medicine preparation) is the collection of illustrative plates that reflects this Chinese medicine feature, identifies the total peak of this Chinese medicine characteristic, the kind and the quantity of the contained chemical constitution of Chinese medicine be can reflect more all sidedly, and then the discriminating and the quality control of Chinese medicine carried out.Set up the finger-print of different plant origins or different places of production Chinese medicine, on this basis, by the comparison of correlativity between pharmacodynamics and the finger-print,, seek the foundation of judging its quality good or not according to finger-print provided about the kind of this chemical composition of Chinese materia medica and the information of content.But the report that the utilization infrared spectrum technology detects the Chinese patent drug effective ingredient but seldom.
Summary of the invention
The purpose of this invention is to provide the infrared spectrum technology that a kind of any component concentration that can apply to the Chinese medicine dripping pills preparation detects.
The infrared spectrum detection method of effective constituent in a kind of Chinese medicine dripping pills preparation provided by the invention may further comprise the steps:
1) infrared spectrum technology, the infrared spectrum of any known component of measurement Chinese medicine dripping pills;
2) after the infrared spectrum to this component carries out pre-service, set up the quantitative relationship of absorbance and this component concentration of this component, set up quantitative math-model;
3) to the same component of content not record its infrared spectrum and the above-mentioned mathematical model of substitution, by calculating this components contents.
One of detection method of the present invention is: at the infrared spectrum of near infrared region utilization scattered reflection or transmitted spectrum commercial measurement sample.The wave band that adopts is 10000-4000cm
-1The preferred bands scope is: 5800-5500cm
-1, 8600-8000cm
-1
The present invention in one of measuring method of near infrared region test sample absorbance is: Chinese medicine dripping pills is dissolved as liquid with chloroform, utilization scattered reflection or transmitted spectrum technology, the infrared spectrum of measuring samples.
The present invention in two of the measuring method of near infrared region test sample absorbance is: Chinese medicine dripping pills is made section, utilization scattered reflection or transmitted spectrum technology, the infrared spectrum of measuring samples.
Two of detection method of the present invention is: at the infrared spectrum of mid infrared region utilization ATR spectral technique or transmitted spectrum commercial measurement sample.The wave band that adopts is 4000-300cm
-1The preferred bands scope is: 3300-3500cm
-1, 2950-2970cm
-1, 1460-1490cm
-1, 1380-1400cm
-1, 1070-1045cm
-1
The present invention in one of measuring method of mid infrared region test sample absorbance is: Chinese medicine dripping pills is made section, adopt the infrared spectrum of ATR spectral technique or transmitted spectrum commercial measurement sample.When adopting the ATR spectral technique to measure, with CO
2Gas is at 2350cm
-1The absorbance at place is a standard, and the absorbance of sample is done normalized, eliminates solid sample and contacts not closely the air-gap of generation with atr crystal to the influence of measurement result.
The present invention in two of the measuring method of mid infrared region test sample absorbance is: after Chinese medicine dripping pills is dissolved as liquid with chloroform, and the infrared spectrum of utilization ATR spectroscopy measurement sample.In the measurement with chloroformic solution at 1215cm
-1The absorbance at place is a standard, and the absorbance of sample is done normalized.The method that dissolving is measured has avoided problem in the section measurement, the problem includes: the air-gap problem has improved the sensitivity that detects.
The present invention selects solvent chloroform dissolving Chinese medicine dripping pills for use.Near the absorbance of the chloroform characteristic absorption peak of borneol is almost nil, the overlapping influence to detectability of absorption peak has been dropped to minimum, has improved the signal to noise ratio (S/N ratio) of measuring; Simultaneously sample is had solubility preferably, avoided of the influence of undissolved suspended particle accuracy of detection.Get ball and heavily be the 40mg/ grain, wherein the mark vector of content of bornyl alcohol is the Chinese medicine dripping pills of 6mg ± 10%, and the concentration range of dissolving is: 1/20ml-100 grain/20ml; Preferable range is 2/20ml-50 grain/20ml.
The present invention has adopted normalized preprocess method to eliminate The noise when ir data is handled.
The present invention is suitable for the apparatus that infrared spectrum detection method constituted of effective constituent in any Chinese medicine dripping pills preparation.
Embodiment
Below further specify the present invention with example.
Example is that the sample series with complex background composition that content of bornyl alcohol changes is in gradient carried out Infrared spectroscopy.
Experiment selects that foremost product suxiao jiuxin pills is an application example in the Chinese medicine dripping pills for use.This kind is the 40mg/ grain, and wherein the mark vector of content of bornyl alcohol is 6mg ± 10%.Because in process of production, borneol volatilizees easily, and it is not very accurate making the content in the production run, behind finished product, test, and defective will scrapping, this method can be carried out the production on-line measurement, detects and regulate content at any time, brings great convenience to production.
In specimen preparation, with the chloroformic solution of suxiao jiuxin pills as mother liquor, the ball of considering every of suxiao jiuxin pills heavily is not identical utterly, in order to guarantee the consistance of various sample mother liquid concentration, when specimen preparation, get ball and heavily be the 40mg/ grain, wherein the mark vector of content of bornyl alcohol is that 200 suxiao jiuxin pillses of suxiao jiuxin pills of 6mg ± 10% are dissolved in chloroform, and be 100ml with the solution constant volume, after this concentration value was demarcated with liquid chromatography, the concentration of borneol was 12.0267mg/ml in the solution.To each sample, get the mother liquor 2ml of same amount, add the borneols of different amounts respectively, the theoretical value that adds borneol is: 1,2,3,4,5,7,8,10,12,13,14,15,16,17,18,19,20,21,23,25,27,29,30,32 (unit is: mg).Be 10ml with chloroform with each sample constant volume at last.
Choose wavelength band: 2950-2970cm
-1, 1460-1490cm
-1And 1380-1400cm
-1
The infrared spectrum of the sample that experiment is obtained adopts above-mentioned wave band to carry out modeling and forecasting.Pretreated method is normalization, promptly with chloroformic solution at 1215cm
-1The absorbance at place is a standard, and the absorbance of sample is done normalized.The result of modeling and forecasting evaluation index is: (mg/10ml)=0.913857, related coefficient is 0.995841 to predicated error root mean square (Root Mean Squareof Prediction is abbreviated as RMSEP), and number of principal components is 5.Modeling and forecasting the results are shown in Table 1.
The relative error value of table 1 experimental result
Sample number chromatogram value spectral value relative error Number of samples Reference Data Predictive Data Relative Errors
1 25.045 25.185 0.56％
2 26.034 26.136 0.39％
3 27.024 26.349 -2.50％
4 28.013 27.383 -2.25％
5 29.003 28.260 -2.56％
7 30.982 32.042 3.42％
8 31.971 32.375 1.26％
10 33.950 35.408 4.30％
12 35.312 35.556 0.69％
13 36.919 36.196 -1.96％
14 37.908 38.137 0.60％
15 38.898 38.627 -0.70％
16 39.887 39.354 -1.34％
17 40.877 40.286 -1.45％
18 41.866 42.155 0.69％
19 42.856 44.303 3.38％
20 43.845 42.446 -3.19％
21 44.835 44.219 -1.37％
23 46.814 46.730 -0.18％
25 48.793 47.682 -2.28％
27 50.772 50.602 -0.34％
29 52.751 54.657 3.61％
30 53.740 52.289 -2.70％
32 55.719 55.901 0.33％
By the relative error value in the table 1 as can be seen, utilization middle infrared spectrum detection technique detects content of bornyl alcohol in the Chinese patent drug suxiao jiuxin pills, and the maximum relative error value is 4.30% only, satisfies the requirement that commercial production detects index.Use the content that the present invention detects one of Chinese medicine dripping pills effective constituent borneol, the relative error value of its testing result not only can reach the present commercial production relative error scope that control is allowed to content of bornyl alcohol, and the maximum error value that will allow much smaller than present commercial production, for the present invention be applied to the production of Chinese medicine dripping pills suxiao jiuxin pills line Quality Control, change in the present commercial production breakthrough progress played in the empirical control of content of bornyl alcohol.
The present invention discloses and has proposed detection method, although method of the present invention and detect active principle with the method and be described by preferred embodiment, person skilled obviously can change or reconfigure method as herein described and technology path in not break away from content of the present invention, spirit and scope, realizes the present invention.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as being included in spirit of the present invention, scope and the content.
Claims (12)
1. the infrared spectrum detection method of effective constituent in the Chinese medicine dripping pills preparation is characterized in that:
1) external spectrum technology, the infrared spectrum of any known component of measurement Chinese medicine dripping pills;
2) after the infrared spectrum to this component carries out pre-service, set up the quantitative relationship of absorbance and this component concentration of this component, set up quantitative math-model;
3) to the same component of content not record its infrared spectrum and the above-mentioned mathematical model of substitution, by calculating this components contents.
2. the infrared spectrum detection method of effective constituent in a kind of Chinese medicine dripping pills preparation as claimed in claim 1 is characterized in that described component is a borneol.
3. the infrared spectrum detection method of effective constituent in a kind of Chinese medicine dripping pills preparation as claimed in claim 1 or 2, it is characterized in that described borneol component infrared spectrum detection method is: the employing wave band is 10000-4000cm
-1At near infrared region, Chinese medicine dripping pills is dissolved as liquid with chloroform, the infrared spectrum of utilization scattered reflection or transmitted spectrum commercial measurement sample.
4. the infrared spectrum detection method of effective constituent in a kind of Chinese medicine dripping pills preparation as claimed in claim 1 or 2, it is characterized in that described borneol component infrared spectrum detection method is: the employing wave band is 10000-4000cm
-1At near infrared region, Chinese medicine dripping pills is made section, utilization scattered reflection or transmitted spectrum technology, the infrared spectrum of measuring samples.
5. as the infrared spectrum detection method of effective constituent in claim 3 or the 4 described a kind of Chinese medicine dripping pills preparations, it is characterized in that: described wave band is 5800-5500cm
-1, 8600-8000cm
-1
6. the infrared spectrum detection method of effective constituent in a kind of Chinese medicine dripping pills preparation as claimed in claim 1 or 2, it is characterized in that described borneol component infrared spectrum detection method is: at the infrared spectrum of mid infrared region utilization ATR spectral technique or transmitted spectrum commercial measurement sample, the wave band of employing is 4000-300cm
-1Chinese medicine dripping pills is made section, adopt the infrared spectrum of ATR spectral technique or transmitted spectrum commercial measurement sample; When adopting the ATR spectral technique to measure, with CO
2Gas is at 2350cm
-1The absorbance at place is a standard, and the absorbance of sample is done normalized, eliminates solid sample and contacts not closely the air-gap of generation with atr crystal to the influence of measurement result.
7. the infrared spectrum detection method of effective constituent in a kind of Chinese medicine dripping pills preparation as claimed in claim 1 or 2, it is characterized in that described borneol component infrared spectrum detection method is: in mid infrared region, after Chinese medicine dripping pills is dissolved as liquid with chloroform, the infrared spectrum of utilization ATR spectroscopy measurement sample, the wave band of employing is 4000-300cm
-1In the measurement with chloroformic solution at 1215cm
-1The absorbance at place is a standard, and the absorbance of sample is done normalized; The method that dissolving is measured has avoided problem in the section measurement, the problem includes: the air-gap problem has improved the sensitivity that detects.
8. as the infrared spectrum detection method of effective constituent in claim 6 or the 7 described a kind of Chinese medicine dripping pills preparations, it is characterized in that: described wavelength band is: 3300-3500cm
-1, 2950-2970cm
-1, 1460-1490cm
-1, 1380-1400cm
-1, 1070-1045cm
-1
9. the infrared spectrum detection method of borneol composition in the pills for curing heart disease preparation is characterized in that: measure each standard model at wave band 2950-2970cm with infrared spectrometer
-1, 1460-1490cm
-1And 1380-1400cm
-1The infrared spectrum at characteristic absorption peak place; After the normalization pre-service, set up the model of the mathematical relation of absorbance and content of bornyl alcohol; Get ball heavily for the 40mg/ grain, wherein the mark vector of content of bornyl alcohol is the suxiao jiuxin pills of 6mg ± 10%, with the matched proportion density scope of chloroform is: 1/20ml-100 grain/20ml; Directly measure the infrared spectrum of this sample, just can obtain the content of borneol in this sample with the mathematical model of building up.
10. the infrared spectrum detection method of borneol composition in a kind of pills for curing heart disease preparation as claimed in claim 9 is characterized in that the proportioning of described suxiao jiuxin pills and chloroform concentration is: 2/20ml-50 grain/20ml.
11. the infrared spectrum detection method of borneol composition in a kind of pills for curing heart disease preparation as claimed in claim 9, it is characterized in that it is 0.913857 that described mathematical model modeling and forecasting evaluation index adopts predicated error root mean square, related coefficient is 0.995841, and number of principal components is 5.
12. the infrared spectrum detection method of effective constituent in the Chinese medicine dripping pills preparation is characterized in that being suitable for the apparatus that infrared spectrum detection method constituted of effective constituent in any Chinese medicine dripping pills preparation.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1982873B (en) * | 2005-12-16 | 2010-08-11 | 天津天士力制药股份有限公司 | Near-infrared diffuse reflection spectral method for fastly inspecting drop appearance quality |
| CN1982874B (en) * | 2005-12-16 | 2010-08-11 | 天津天士力制药股份有限公司 | Near-infrared diffuse reflection spectral method for fastly inspecting drop effective ingredient content |
| CN1982872B (en) * | 2005-12-16 | 2010-09-29 | 天津天士力制药股份有限公司 | Near-infrared diffuse reflection spectral method for fastly inspecting drop water content |
| CN105043995A (en) * | 2015-04-23 | 2015-11-11 | 天津大学 | Position sine save frequency encoded array-type transmission light measurement system |
| CN107655848A (en) * | 2017-09-29 | 2018-02-02 | 安徽同心化工有限公司 | The method for building up of the detection method of antioxidant content and its detection model in a kind of Petropols |
| CN107941744A (en) * | 2017-11-16 | 2018-04-20 | 广州白云山和记黄埔中药有限公司 | Quickly judge the method for borneol uniformity and application in Fufang Danshen Pian production process |
| CN108240974A (en) * | 2017-12-22 | 2018-07-03 | 无锡济民可信山禾药业股份有限公司 | A kind of natural borneol near infrared spectrum detection method |
| CN110785661A (en) * | 2017-04-21 | 2020-02-11 | 英索特有限公司 | Method for detecting rancidity in oil-containing fruits, seeds and nuts |
-
2002
- 2002-12-31 CN CN 02159972 patent/CN1425909A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1982873B (en) * | 2005-12-16 | 2010-08-11 | 天津天士力制药股份有限公司 | Near-infrared diffuse reflection spectral method for fastly inspecting drop appearance quality |
| CN1982874B (en) * | 2005-12-16 | 2010-08-11 | 天津天士力制药股份有限公司 | Near-infrared diffuse reflection spectral method for fastly inspecting drop effective ingredient content |
| CN1982872B (en) * | 2005-12-16 | 2010-09-29 | 天津天士力制药股份有限公司 | Near-infrared diffuse reflection spectral method for fastly inspecting drop water content |
| CN105043995A (en) * | 2015-04-23 | 2015-11-11 | 天津大学 | Position sine save frequency encoded array-type transmission light measurement system |
| CN110785661A (en) * | 2017-04-21 | 2020-02-11 | 英索特有限公司 | Method for detecting rancidity in oil-containing fruits, seeds and nuts |
| CN107655848A (en) * | 2017-09-29 | 2018-02-02 | 安徽同心化工有限公司 | The method for building up of the detection method of antioxidant content and its detection model in a kind of Petropols |
| CN107941744A (en) * | 2017-11-16 | 2018-04-20 | 广州白云山和记黄埔中药有限公司 | Quickly judge the method for borneol uniformity and application in Fufang Danshen Pian production process |
| CN108240974A (en) * | 2017-12-22 | 2018-07-03 | 无锡济民可信山禾药业股份有限公司 | A kind of natural borneol near infrared spectrum detection method |
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