CN104730023A - Method for establishing quantitative model of auxiliary materials of Chinese medicinal granules - Google Patents
Method for establishing quantitative model of auxiliary materials of Chinese medicinal granules Download PDFInfo
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- CN104730023A CN104730023A CN201510104623.8A CN201510104623A CN104730023A CN 104730023 A CN104730023 A CN 104730023A CN 201510104623 A CN201510104623 A CN 201510104623A CN 104730023 A CN104730023 A CN 104730023A
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Abstract
The invention discloses a method for establishing a quantitative model of auxiliary materials of Chinese medicinal granules. The method comprises the following steps: (1) acquiring infrared spectra of the Chinese medicinal granules of auxiliary materials with different proportions, and establishing different model samples so as to form a model database; (2) comparing parameters of the model samples at different sensitive wave number bands, and screening quantitative wave number bands; (3) verifying the wave number section models with relatively excellent parameters, and enabling the wave number bands of the verified result to be corresponding parameters of the quantitative models; and (4) predicting the content of the auxiliary materials of a plurality of Chinese medicinal granules by the quantitative models, and comparing the predicted result with the content of known auxiliary materials so as to determine the parameters of the final quantitative model. The method is used for quantifying the auxiliary materials in the Chinese medicinal granules by utilizing an infrared technique, and the established auxiliary quantitative model can simply and rapidly determine the auxiliary material adding amount in the Chinese medicinal granules, and an important means is provided for evaluating the quality of the Chinese medicinal granules.
Description
[technical field]
The present invention relates to Pharmaceutical Analysis technical field, particularly measure the analytical technology of pharmaceutical compositions content with infrared ray.
[background technology]
Chinese medicinal granule is on the basis of following theory of traditional Chinese medical science, and with meeting, to concoct the prepared slices of Chinese crude drugs required be raw material, concentrate through industrialized extraction, dry, to granulate and the technological process such as point process of assembling refines.According to physicochemical property and the technological requirement of each taste Chinese medicine, part Chinese medicinal granule needs to add suitable auxiliary material in preparation process, and therefore, the addition of auxiliary material can have influence on the quality of Chinese medicinal granule.Monitoring means at present for auxiliary material addition in Chinese medicinal granule lack, and easily cause market upper part producer for reaping staggering profits and excessive interpolation auxiliary material.
The principle of infrared spectrum measurement is the absorption spectrum of material Middle molecule, and different materials has the characteristic of its characteristic fingerprint.Chinese medicinal granule is a complicated mixed system, its infrared spectrum is the superposition of its each composition information, the fingerprint characteristic utilizing infrared spectrum to have at present can carry out quality discrimination to Chinese medicinal granule quickly and accurately, holistic approach is carried out to its full constituent, meets the Overall View of differential diagnosis in tcm thinking.
Infrared spectrum technology is combined with Chemical Measurement and can be used for quantitative examination.At present, utilize the near infrared spectrum of sample more, resolve its spectral information, with the characteristic information of the target component extracted for quantitative parameter, and utilize chemometrics method to set up quantitative model, what realize special component is quantitative.The pre-service of the accuracy of near infrared quantitative model and the selection of model parameter, data, sample size, sample contain the comprehensive relevant of information.The near infrared spectrum of material is frequency multiplication and the sum of fundamental frequencies absorption of hydric group vibration, the overlapping of its near-infrared spectra district spectrum and uncontinuity, the information relevant to component content in material near infrared spectrum is difficult to extracting directly out, for beginner or infrared relevant knowledge deficient patients, quantitative parameter be selected to the biggest problem that it sets up quantitative model.At present, utilize infrared technique to determine quantifier elimination to auxiliary material less, rarely have report especially about auxiliary material near infrared quantitative technique.
[summary of the invention]
Based on the above-mentioned defect of the prior art of improvement, the object of the invention is to for the deficiencies in the prior art and actual needs, provide a kind of method for building up of Chinese medicinal granule auxiliary material quantitative model, instruct the foundation of Chinese medicinal granule auxiliary material infrared quantitative model, utilize the monitoring of auxiliary material quantitative model realization to auxiliary material addition in Chinese medicinal granule, control the quality of Chinese medicinal granule comprehensively.
The method for building up of a kind of Chinese medicinal granule auxiliary material quantitative model that the present invention proposes, comprises the following step:
Step 1: the infrared spectrum obtaining the Chinese medicinal granule of different proportion auxiliary material, sets up different model sample according to described auxiliary material proportion contained in described different Chinese medicinal granule;
Step 2: the parameter of more described model sample, selects described model sample and verifies, according to the relevant parameter of the result as described Chinese medicinal granule auxiliary material quantitative model.
Further, the mode selecting model sample in step 2 is that the wave number section of the infrared spectrum of Chinese medicinal granule according to different proportion auxiliary material is screened.
Further, also include step 3: utilize quantitative model to carry out auxiliary material content prediction to many batches of Chinese medicinal granules containing auxiliary material, will predict the outcome and to compare with well known auxiliaries content, to adjust the parameter of quantitative model.
Further, in abovementioned steps 3, if comparison result differs greatly, model sample need be increased and repeat step 2 ~ step 3.
Further, according to the parameter of the wave number section of auxiliary material increase and decrease sensitivity in infrared spectrum as model sample in step 1, with the difference of the Chinese medicinal granule infrared spectrum containing different proportion auxiliary material for dependent variable, auxiliary material is independent variable Modling model sample.
Further, the difference of aforementioned Chinese medicinal granule infrared spectrum is the difference of peak area, peak height or spectral shape.
Further, in step 2, the parameter of model sample comprises performance index, correction error root mean square, predicated error root mean square.
Further, infrared spectrum can be original spectrum or through pretreated spectrum.
Further, aforementioned pretreated method comprises smoothing processing, baseline correction, Baseline Survey, asks different process, normalization process.
Further, model sample can utilize and be mixed with the pure extract powder standard diagram in infrared data storehouse and the most close a collection of or many batches of pure extract powders of auxiliary material standard diagram and auxiliary material.
The Chinese medicinal granule auxiliary material quantitative model utilizing the present invention to set up, meets the overall control overflow of Chinese medicinal granule, and what can realize auxiliary material is quantitative; And model is through methodological study, ensure the accuracy of measurement result; Meanwhile, intuitively simple for the selection of quantitative parameter in the present invention, low to the requirement of the infrared knowledge of modeling personnel, do not need correlation experience.
[accompanying drawing explanation]
Fig. 1 is the flow chart of steps of quantitative model method for building up of the present invention.
The pure extract powder infrared spectrogram of Fig. 2 red sage root.
Fig. 3 dextrin infrared spectrogram.
Fig. 4 model related coefficient figure.
[embodiment]
Because the present invention mainly discloses a kind of method for building up of Chinese medicinal granule auxiliary material quantitative model, the wherein making knowledge of involved Chinese medicinal granule, usually know that the knowledgeable can understand for correlative technology field has, therefore with explanation hereinafter, no longer do complete description.Meanwhile, with hereinafter contrast graphic, only express the signal relevant with feature of the present invention, formerly illustrate.
Chinese medicinal granule auxiliary material quantitative model method for building up of the present invention, mainly comprises following steps:
Step 1: the infrared spectrum obtaining the Chinese medicinal granule of different proportion auxiliary material, sets up different model sample according to described auxiliary material proportion contained in described different Chinese medicinal granule;
Step 2: the parameter of more described model sample, selects described model sample and verifies, according to the relevant parameter of the result as described Chinese medicinal granule auxiliary material quantitative model.
Specific operation process please refer to Fig. 1, and method is as follows:
(1) infrared spectrum of the Chinese medicinal granule of different proportion auxiliary material is obtained, according to the wave number section of auxiliary material increase and decrease sensitivity in infrared spectrum as model parameter, with the difference of the Chinese medicinal granule infrared spectrum containing different proportion auxiliary material for dependent variable, auxiliary material is independent variable, partial least square method regression model is adopted to set up different model sample, formation model database, the difference of Chinese medicinal granule infrared spectrum can be the difference of peak area, peak height or spectral shape; Wherein, infrared spectrum is original spectrum or through pretreated spectrum, the method for spectral manipulation can comprise smoothing processing, baseline correction, Baseline Survey, asks the mode such as different process, normalization process;
(2) parameters of model sample set up of more different responsive wave number section, such as comprise performance index, correction error root mean square (RMSEC) and related coefficient thereof, predicated error root mean square (RMSEP) and related coefficient thereof etc., and quantitative wave number section is screened;
(3) Selection parameter preferably wave number segment model verify, and select the wave number section of the result to be the relevant parameter of quantitative model; The mode of checking adopts the mode of methodological study, and side comprises repeatability, accurate Du, average recovery, detectability, quantitative limit etc.;
(4) quantitative model is utilized to carry out auxiliary material content prediction to the many batches of Chinese medicinal granules containing auxiliary material, wherein comprise the auxiliary material of different Ji Yuan, Different sources, and will predict the outcome and to compare with well known auxiliaries content, if comparison result differs greatly, the sample in model database need be increased, and repeat step 2 ~ step 4, to confirm final quantitative model, if result difference is less, such as result uncertainty is less than 20%, then judgment models can be used, and completes the foundation of model.
Key is in the present invention the screening of quantitative parameter, first by observing the infared spectrum of the Chinese medicinal granule containing different proportion auxiliary material, search out sensitive quantitation wave number section, then tentatively sensitive quantitation wave number section is screened by model evaluation dependence on parameter, RMSEC, then the quantitative parameter determining final quantitative model is investigated by method, and compared by sample prediction, auxiliary material quantitative model is adjusted.
In order to make the present invention be easier to understand, specific embodiment of the invention will be set forth further below.
embodiment
The present embodiment is the foundation of Danshen formula particles auxiliary material infrared quantitative model, and concrete steps are as follows:
1) the pure extract powder of a collection of qualified red sage root and dextrin in Fig. 2,3 is chosen respectively, precision takes a certain amount of pure medicinal extract fine powder and dextrin fine powder, mix, make the content containing dextrin in its potpourri be 0 ~ 100%, preparation total amount is totally 200 parts, the sample of about 1.00g.Gather the infrared spectrum of above-mentioned sample, the relatively difference of its infrared spectrum, using in spectrum with the more sensitive wave number section 1800cm-1-700cm-1 of auxiliary material increase and decrease, 1800cm-1-1550cm-1,1550cm-1-1200cm-1,1180cm-1-1130cm-1,1130cm-1-945cm-1,945cm-1-700cm-1 as quantitative model parameter, with the difference of the Chinese medicinal granule infrared spectrum containing different proportion auxiliary material for dependent variable, auxiliary material proportion is independent variable, adopt partial least square method to set up regression model, see Fig. 4.
2) parameter such as RMSEC, related coefficient of more above-mentioned wave number segment model, carries out preliminary screening to quantitative wave number section.
Table 1 model performance index
3) by carrying out methodological study to the model of the more excellent wave number section of parameter, methodological study comprises repeatability, precision, average recovery, detectability, quantitative limit, and is defined as the final mask parameter of Chinese medicinal granule auxiliary material infrared quantitative model for 945cm-1-700cm-1 with the wave number section of optimum the result.
Table 2 methodological study result
| Wave number section | Precision | Repeatability/% | Average recovery/% |
| 1800cm-1-700cm-1 | 1.57～11.39 | 1.57～2.31 | 94.82～124.07 |
| 945cm-1-700cm-1 | 2.6～6.29 | 0.86～1.29 | 93.27～102.02 |
4) have collected the pure extract powder of the red sage root of Shanxi, Shandong, Gansu, Baoding Different sources respectively, according to step 1) carry out the acquisition of sample preparation, infrared spectrum, and bring infrared spectrum information into quantitative model and predict, to predict the outcome and to compare with well known auxiliaries content, result uncertainty is less than 20%, and model has been set up.
Table 3 predicts the outcome
| Wave number section | Predict the outcome uncertainty/% |
| Shanxi | 1.00～8.69 |
| Shandong | 1.67～16.89 |
| Gansu | 0.17～9.36 |
| Baoding | 1.02～5.67 |
Claims (8)
1. a method for building up for Chinese medicinal granule auxiliary material quantitative model, is characterized in that comprising the following step:
Step 1: the infrared spectrum obtaining the Chinese medicinal granule of different proportion auxiliary material, sets up different model sample according to described auxiliary material proportion contained in described different Chinese medicinal granule;
Step 2: the parameter of more described model sample, selects described model sample and verifies, according to the relevant parameter of the result as described Chinese medicinal granule auxiliary material quantitative model.
2. the method for building up of Chinese medicinal granule auxiliary material quantitative model according to claim 1, it is characterized in that, in described step 2, the mode selecting described model sample is that the wave number section of the infrared spectrum of Chinese medicinal granule according to described different proportion auxiliary material is screened.
3. the method for building up of Chinese medicinal granule auxiliary material quantitative model according to claim 1, it is characterized in that, comprise step 3 further: utilize described quantitative model to carry out auxiliary material content prediction to the many batches of Chinese medicinal granules containing described auxiliary material, described predicting the outcome is compared with known described auxiliary material content, to adjust the parameter of described quantitative model.
4. the method for building up of Chinese medicinal granule auxiliary material quantitative model according to claim 3, is characterized in that: in described step 3, if comparison result differs greatly, need increase described model sample, and repeating said steps 2 ~ step 3.
5. the method for building up of Chinese medicinal granule auxiliary material quantitative model according to claim 1, it is characterized in that, according to the parameter of the wave number section of the sensitivity of auxiliary material increase and decrease described in described infrared spectrum as described model sample in step 1, with the difference of the Chinese medicinal granule infrared spectrum containing auxiliary material described in different proportion for dependent variable, described auxiliary material is that independent variable sets up described model sample.
6. the method for building up of Chinese medicinal granule auxiliary material quantitative model according to claim 5, is characterized in that: the difference of described Chinese medicinal granule infrared spectrum is the difference of peak area, peak height or spectral shape.
7. the method for building up of Chinese medicinal granule auxiliary material quantitative model according to claim 1, is characterized in that: the parameter of the sample of model described in step 2 comprises performance index, correction error root mean square, predicated error root mean square.
8. the method for building up of Chinese medicinal granule auxiliary material quantitative model according to claim 1, is characterized in that: described infrared spectrum can be original spectrum or through pretreated spectrum.
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Cited By (4)
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| CN106404710A (en) * | 2015-07-15 | 2017-02-15 | 重庆医科大学 | Pharmaceutical powder auxiliary material near-infrared spectrum rapid non-destructive identification method |
| CN107179293A (en) * | 2017-06-23 | 2017-09-19 | 南京富岛信息工程有限公司 | A kind of assessment method of oil property uncertainty |
| CN107505282A (en) * | 2017-08-28 | 2017-12-22 | 南京富岛信息工程有限公司 | A kind of method for improving oil product near-infrared modeling robustness |
| CN111141862A (en) * | 2019-12-31 | 2020-05-12 | 广州汇标检测技术中心 | Method for detecting butyric acid in feed |
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| CN101299022A (en) * | 2008-06-20 | 2008-11-05 | 河南中医学院 | Method for evaluating Chinese medicine comprehensive quality using near infrared spectra technique |
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| CN106404710A (en) * | 2015-07-15 | 2017-02-15 | 重庆医科大学 | Pharmaceutical powder auxiliary material near-infrared spectrum rapid non-destructive identification method |
| CN107179293A (en) * | 2017-06-23 | 2017-09-19 | 南京富岛信息工程有限公司 | A kind of assessment method of oil property uncertainty |
| CN107505282A (en) * | 2017-08-28 | 2017-12-22 | 南京富岛信息工程有限公司 | A kind of method for improving oil product near-infrared modeling robustness |
| CN111141862A (en) * | 2019-12-31 | 2020-05-12 | 广州汇标检测技术中心 | Method for detecting butyric acid in feed |
| CN111141862B (en) * | 2019-12-31 | 2022-12-02 | 广州汇标检测技术中心 | Method for detecting butyric acid in feed |
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Inventor after: Zhang Zhiqiang Inventor after: Fu Jing Inventor after: Shen Jianmei Inventor after: Chen Jingran Inventor before: Shen Jianmei Inventor before: Chen Jingran |
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