CN111380832A - Method for constructing and detecting compound liquorice tablet effective component content determination correction model - Google Patents
Method for constructing and detecting compound liquorice tablet effective component content determination correction model Download PDFInfo
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- LPLVUJXQOOQHMX-QWBHMCJMSA-N glycyrrhizinic acid Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@@H]1C([C@H]2[C@]([C@@H]3[C@@]([C@@]4(CC[C@@]5(C)CC[C@@](C)(C[C@H]5C4=CC3=O)C(O)=O)C)(C)CC2)(C)CC1)(C)C)C(O)=O)[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O LPLVUJXQOOQHMX-QWBHMCJMSA-N 0.000 title claims abstract description 110
- 238000012937 correction Methods 0.000 title claims abstract description 80
- 150000001875 compounds Chemical class 0.000 title claims abstract description 79
- 235000006200 Glycyrrhiza glabra Nutrition 0.000 title claims abstract description 78
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- 235000011477 liquorice Nutrition 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 43
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- LPLVUJXQOOQHMX-UHFFFAOYSA-N glycyrrhetinic acid glycoside Natural products C1CC(C2C(C3(CCC4(C)CCC(C)(CC4C3=CC2=O)C(O)=O)C)(C)CC2)(C)C2C(C)(C)C1OC1OC(C(O)=O)C(O)C(O)C1OC1OC(C(O)=O)C(O)C(O)C1O LPLVUJXQOOQHMX-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229960004949 glycyrrhizic acid Drugs 0.000 claims abstract description 39
- UYRUBYNTXSDKQT-UHFFFAOYSA-N glycyrrhizic acid Natural products CC1(C)C(CCC2(C)C1CCC3(C)C2C(=O)C=C4C5CC(C)(CCC5(C)CCC34C)C(=O)O)OC6OC(C(O)C(O)C6OC7OC(O)C(O)C(O)C7C(=O)O)C(=O)O UYRUBYNTXSDKQT-UHFFFAOYSA-N 0.000 claims abstract description 39
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- 239000012071 phase Substances 0.000 description 3
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 description 2
- KSDSYIXRWHRPMN-UHFFFAOYSA-N 4'-O-beta-D-Galactopyranoside-6''-p-Coumaroylprunin-4',5,7-Trihydroxyflavanone Natural products OC1C(O)C(O)C(CO)OC1OC1=CC=C(C2OC3=CC(O)=CC(O)=C3C(=O)C2)C=C1 KSDSYIXRWHRPMN-UHFFFAOYSA-N 0.000 description 2
- 241000723346 Cinnamomum camphora Species 0.000 description 2
- 206010011224 Cough Diseases 0.000 description 2
- DEMKZLAVQYISIA-ONJCETCRSA-N Liquiritin Natural products O([C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1)c1ccc([C@@H]2Oc3c(C(=O)C2)ccc(O)c3)cc1 DEMKZLAVQYISIA-ONJCETCRSA-N 0.000 description 2
- DEMKZLAVQYISIA-UHFFFAOYSA-N Liquirtin Natural products OC1C(O)C(O)C(CO)OC1OC1=CC=C(C2OC3=CC(O)=CC=C3C(=O)C2)C=C1 DEMKZLAVQYISIA-UHFFFAOYSA-N 0.000 description 2
- 239000008896 Opium Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
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- OROGSEYTTFOCAN-DNJOTXNNSA-N codeine Chemical compound C([C@H]1[C@H](N(CC[C@@]112)C)C3)=C[C@H](O)[C@@H]1OC1=C2C3=CC=C1OC OROGSEYTTFOCAN-DNJOTXNNSA-N 0.000 description 2
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- DEMKZLAVQYISIA-ZRWXNEIDSA-N liquiritin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC=C([C@H]2OC3=CC(O)=CC=C3C(=O)C2)C=C1 DEMKZLAVQYISIA-ZRWXNEIDSA-N 0.000 description 2
- 229960005181 morphine Drugs 0.000 description 2
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 description 2
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- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 2
- 235000010234 sodium benzoate Nutrition 0.000 description 2
- 239000004299 sodium benzoate Substances 0.000 description 2
- GSZUGBAEBARHAW-UHFFFAOYSA-N sophoraflavone B Natural products OC1C(O)C(O)C(CO)OC1OC1=CC=C(C=2OC3=CC(O)=CC=C3C(=O)C=2)C=C1 GSZUGBAEBARHAW-UHFFFAOYSA-N 0.000 description 2
- 208000024794 sputum Diseases 0.000 description 2
- 210000003802 sputum Anatomy 0.000 description 2
- 238000010561 standard procedure Methods 0.000 description 2
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- 239000000126 substance Substances 0.000 description 2
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- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
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- 240000001090 Papaver somniferum Species 0.000 description 1
- 235000008753 Papaver somniferum Nutrition 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000000954 anitussive effect Effects 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 229940124584 antitussives Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229940045348 brown mixture Drugs 0.000 description 1
- 229960004126 codeine Drugs 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- ZZVUWRFHKOJYTH-UHFFFAOYSA-N diphenhydramine Chemical compound C=1C=CC=CC=1C(OCCN(C)C)C1=CC=CC=C1 ZZVUWRFHKOJYTH-UHFFFAOYSA-N 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
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- 239000003172 expectorant agent Substances 0.000 description 1
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- 230000000762 glandular Effects 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- OROGSEYTTFOCAN-UHFFFAOYSA-N hydrocodone Natural products C1C(N(CCC234)C)C2C=CC(O)C3OC2=C4C1=CC=C2OC OROGSEYTTFOCAN-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
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- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 1
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- 208000026435 phlegm Diseases 0.000 description 1
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
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- 210000001533 respiratory mucosa Anatomy 0.000 description 1
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- REFMEZARFCPESH-UHFFFAOYSA-M sodium;heptane-1-sulfonate Chemical compound [Na+].CCCCCCCS([O-])(=O)=O REFMEZARFCPESH-UHFFFAOYSA-M 0.000 description 1
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- 229940095064 tartrate Drugs 0.000 description 1
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Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/27—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using photo-electric detection ; circuits for computing concentration
- G01N21/274—Calibration, base line adjustment, drift correction
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
Abstract
The invention provides a method for constructing and detecting a correction model for determining the content of effective components of compound liquorice tablets. The construction comprises the following steps: taking a plurality of compound liquorice tablet samples as a correction set, and scanning by near infrared light to obtain original spectral data of the correction set; performing spectrum preprocessing on the original spectrum data of the correction set, selecting a modeling waveband of the effective component, and acquiring a content characteristic spectrum of the effective component; respectively measuring the effective components of multiple compound liquorice tablet samples contained in the correction set by adopting a high performance liquid chromatography to obtain the true content values of the effective components; and correlating the obtained content characteristic spectrum and the content true value by using a partial least square method, and establishing a content correction model of the effective component. The content correction model is used for detecting the content of glycyrrhizic acid in the compound liquorice tablets: background noise and physical factor dryness can be effectively eliminated, the prediction capability is good, and the detection result is accurate; meanwhile, the content correction model also has strong applicability.
Description
Technical Field
The invention belongs to the technical field of traditional Chinese medicine detection, and particularly relates to a method for constructing and detecting a correction model for determining the content of active ingredients of compound liquorice tablets.
Background
The compound liquorice tablets are Brown mixture (Brown mixura) which is introduced from the United states more than 50 years ago and invented by John Brown physicians (1735-. In 1963, Qinghai pharmaceutical factory deleted potassium antimonate tartrate in Brown original prescription and registered compound radix Glycyrrhizae tablet, but compound radix Glycyrrhizae oral liquid is still used. The prescription of the compound liquorice tablet is changed to that each tablet contains 112.5mg of liquorice extract powder, 4mg of opium powder/poppy fruit extract, 2mg of camphor, 2mg of star anise oil and 2mg of sodium benzoate. It has determined curative effect, low cost and high safety.
The Glycyrrhrizae radix extract in the compound Glycyrrhrizae radix tablet is protective antitussive and expectorant; the opium powder can effectively relieve cough (the drug-effect substances mainly comprise morphine and codeine); the camphor and the star anise oil can stimulate bronchial mucosa, reflectively increase glandular secretion, dilute sputum and facilitate expectoration of the sputum; sodium benzoate is used as antiseptic. The compound preparation composed of the components not only has the effects of relieving cough and eliminating phlegm, but also has certain protective effect on respiratory mucosa.
The existing quality control content measurement of the compound liquorice tablets in Chinese pharmacopoeia at present mainly takes glycyrrhizic acid and morphine as evaluation indexes, and the glycyrrhizic acid content detection method is a high-efficiency liquid phase method, so that complicated pretreatment is often required to a sample, the time and labor are consumed, the measurement time is long, a large amount of reagents are consumed in the detection process, the environmental pollution is large, the physical damage to inspectors is caused, the information feedback is delayed, and the requirements of quick measurement and online detection of multiple batches are difficult to meet in the preparation production.
Near-infrared analysis technology has been widely used for rapid analysis of product quality in various industries as a simple, rapid and nondestructive detection method. For example, the prior art discloses a near infrared spectrum detection method of a licorice medicinal material, which comprises the following steps: pulverizing multiple batches of Glycyrrhrizae radix and sieving; determining content of liquiritin and glycyrrhizic acid in multiple batches of Glycyrrhrizae radix materials by high performance liquid chromatography; collecting near infrared spectrogram of multiple batches of licorice medicinal material powder; the method comprises the steps of adopting near-infrared data in a 5600-10000 cm & lt-1 & gt waveband interval, selecting a first derivative, Savitzky-Golay smoothing and data normalization algorithm to be used for preprocessing the near-infrared spectrum data, and adopting partial least squares regression to establish a quantitative correction model between the near-infrared data and liquiritin and glycyrrhizic acid. However, the effective components of the compound medicament prepared from liquorice are more complex compared with liquorice medicinal materials, and when the effective components of the compound medicament are detected by infrared spectroscopy, the absorption intensity of the characteristic spectral region of the effective components is weak, the signal-to-noise ratio of the spectrum is low, and frequency doubling and combining bands are seriously overlapped, so that the quantitative analysis of NIR spectrum becomes very difficult. Based on the problem, although near infrared analysis for medicinal material detection has been disclosed, no literature report is available for rapidly determining the content of effective components (such as glycyrrhizic acid) in the compound liquorice tablet preparation.
Disclosure of Invention
Based on the above, the main purpose of the invention is to provide a method for constructing a model for measuring the content of the effective components of the compound liquorice tablets. The model for measuring the content of the effective components of the compound liquorice tablets obtained by the construction method can effectively eliminate background noise and physical factor interference, improve the correlation between a spectrogram and target chemical components and has good prediction capability.
The technical purpose of the invention is realized by the following technical scheme:
a construction method of a model for measuring the content of active ingredients of compound liquorice tablets comprises the following steps:
(1) taking a plurality of compound liquorice tablet samples as a correction set, and scanning by near infrared light to obtain original spectral data of the correction set;
(2) performing spectrum preprocessing on the original spectrum data of the correction set, selecting a modeling waveband of the effective component, and acquiring a content characteristic spectrum of the effective component;
(3) respectively measuring the effective components of the multiple compound liquorice tablet samples contained in the correction set by adopting a high performance liquid chromatography to obtain the true content values of the effective components;
(4) correlating the content characteristic spectrum obtained in the step (2) and the content true value obtained in the step (3) by using a partial least square method, and establishing a content correction model of the effective component; the effective component is glycyrrhizic acid.
In one embodiment, step (1) includes performing the following pre-processing on the correction set and then performing the near infrared light scanning: and crushing the correction set compound liquorice tablet sample, sieving the crushed sample with a 50-80-mesh sieve, and drying the sieved part at 60-80 ℃ for 1-5 hours.
In one embodiment, in the step (2), the spectrum preprocessing method is multivariate scattering correction, and the modeling waveband is 4000-10000 cm-1The number of main factors is 7-10.
In one embodiment, in the step (2), the spectrum preprocessing method is multivariate scattering correction, and the modeling waveband is 4000-10000 cm-1The number of main factors is 10.
In one embodiment, the construction method comprises the following steps: taking a plurality of compound liquorice tablet samples as a verification set, preprocessing the samples, and scanning the samples by using near infrared light to obtain original spectral data of the verification set; and importing the original spectrum data of the verification set into the original spectrum data of the verification set for verification.
In one embodiment, the conditions of the near infrared light scan include: resolution ratio of 3-10 cm-1Scanning spectral range of 4000-10000 cm-1The scanning times are 30-35 times, the temperature is 22-28 ℃, and the relative humidity is 32-38%.
In one embodiment, the conditions of the near infrared light scan include: resolution 8cm-1Scanning spectral range of 4000-10000 cm-1The number of scans was 32, 25 ℃ and relative humidity 35%.
The invention also aims to provide a method for detecting the content of the effective components of the compound liquorice tablets, which comprises the following steps:
taking a compound liquorice tablet sample to be detected, preprocessing the sample, and scanning the sample by using near infrared light to obtain original spectral data of the compound liquorice tablet sample to be detected;
inputting the original spectral data of the compound liquorice tablet sample to be detected into a chemometric analysis system of the content correction model constructed by the method, and obtaining the content of the effective components of the compound liquorice tablet sample to be detected through calculation; the effective component is glycyrrhizic acid.
In one embodiment, the compound liquorice tablet to be detected is crushed and sieved by a 50-80-mesh sieve, and then the sieved part is dried for 1-5 hours at the temperature of 60-80 ℃.
In one embodiment, the conditions of the near infrared light scan include: resolution ratio of 3-10 cm-1Scanning spectral range of 4000-10000 cm-1The scanning times are 30-35 times, the temperature is 22-28 ℃, and the relative humidity is 32-38%.
Compared with the prior art, the invention has the following beneficial effects:
based on long-term research on the compound liquorice tablets, the inventor firstly applies the near-infrared analysis technology to the determination of the content of the effective components of the compound liquorice tablets, and particularly applies the near-infrared analysis technology to the determination of the content of glycyrrhizic acid in the compound liquorice tablets by matching with proper sample pretreatment and constructing a content correction model by selecting proper modeling parameters. When the content correction model is adopted to detect the content of glycyrrhizic acid in the compound liquorice tablets: background noise and physical factor interference can be effectively eliminated, a correlation between a spectrogram and the actual content of glycyrrhizic acid is improved, the prediction capability is good, and the detection result is accurate; meanwhile, the content correction model also has strong applicability. In addition, the content measurement by adopting the content correction model also has the following advantages: (1) the analysis speed is high, and the spectral measurement process can be generally completed within 1 minute; (2) the analysis efficiency is high, and a plurality of components or properties of the sample can be simultaneously determined through one-time spectral measurement and the established corresponding correction model; (3) the analysis cost is low, no chemical reagent is needed for near infrared spectrum analysis and detection, the detection cost is greatly reduced, and no pollution is caused to the environment; (4) the test reproducibility is good. Due to the stability of the spectroscopic measurements, the test results are less affected by human factors and the near infrared spectra show better reproducibility than standard or reference methods.
Drawings
FIG. 1, original near infrared spectrum in example 1.
FIG. 2 is a graph of the multivariate scatter corrected spectra in example 1.
Fig. 3 is a comparison graph of the true value and the predicted value of glycyrrhizic acid in the compound licorice tablets in example 1.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The compound liquorice tablets are prepared according to the prescription and the preparation method in the current edition ' compound liquorice tablets ' in pharmacopoeia of the people's republic of China.
Example 1 method for measuring glycyrrhizic acid content in Compound Liquorice tablets
The embodiment provides a method for measuring glycyrrhizic acid content in compound liquorice tablets, which comprises the following steps:
(1) calibration set and raw spectral data acquisition
Collecting 80 batches from the compound liquorice tablets, selecting 60 batches as a correction set, selecting 20 batches as a verification set, crushing the samples, sieving the samples with a 60-mesh sieve, and drying the samples in an oven at 70 ℃ for 3 hours.
Collecting the original spectrum data of the correction set by using a near infrared spectrometer to obtain the original near infrared spectrum data of the compound liquorice tablets, which is shown in figure 1.
A near-infrared spectrometer: antaris II FT-NIR Analyzer Seimer Feishell science, USA, light source; halogen tungsten lamp, detector: InGaAs, integrating sphere diffuse reflection collection system. Resolution 8cm-1Scanning spectral range of 4000-10000 cm-1Number of scans 32 times, room temperature, relative humidity 35%.
(2) Detecting the glycyrrhizic acid content by a high performance liquid chromatograph:
using octadecylsilane chemically bonded silica as filler, 0.025mol/L potassium dihydrogen phosphate solution-0.0025 mol/L sodium heptanesulfonate aqueous solution-acetonitrile (33:33:44) as mobile phase, detecting the wavelength at 250nm, and determining the glycyrrhizic acid content of the sample contained in the correction set of the step (1) according to the glycyrrhizic acid content determination method under item of compound liquorice tablets in pharmacopoeia of the second part of the national pharmacopoeia of the people's republic of China (2015).
(3) Establishing a correction model:
preprocessing the original spectrum data of the correction set obtained in the step (1) to obtain a glycyrrhizic acid content characteristic spectrum in the compound liquorice tablets; establishing a correction model for glycyrrhizic acid in the compound liquorice tablets, establishing the correction model by using Partial Least Squares (PLS) in TQ quantitative analysis software, and performing external verification by using a verification set sample; the glycyrrhizic acid wave band is selected to be 4000-10000 cm-1The spectrum preprocessing method is multivariate scattering correction, and the number of main factors is 10.
In spectral analysis, the general evaluation index of model performance is indicated by a determination coefficient (R)2) Corrected mean square error (RMSEC), verified mean square error (RMSEP). The closer R is to 1, the closer the reference value is to the near-infrared predicted value; the smaller the mean square error is, and the closer the RMSEP and the RMSEC are, the stronger the applicability of the established model is, and the better the prediction effect is.
The original spectral data were preprocessed by multivariate scatter-corrected spectral preprocessing methods, respectively, and the processed spectra are shown in fig. 2, with the results shown in the table.
TABLE 1 glycyrrhizic acid calibration model parameters established by multivariate Scattering calibration method
The glycyrrhizic acid content model is preferably as follows:
① spectrum preprocessing method, multivariate scattering correction
② number of modeling factors 10
③ correlation coefficient (R)2)：0.979
④ corrected mean square error (RMSEC) 0.179
⑤ verification mean square error (RMSEP): 0.197
(4) Prediction of the correction model:
and selecting 20 compound liquorice tablet samples to form a prediction set of a correction model. Collecting the original spectrum data of the prediction set by using a near-infrared spectrometer to obtain the original near-infrared spectrum data of the compound liquorice tablets of the prediction set, inputting the original near-infrared spectrum data into a system imported with an optimal correction model, and calculating to obtain the predicted value of the prediction set; and comparing the predicted value with the true value of the prediction set, and checking the correction model. Wherein the actual value is determined according to the method of step (2).
A near-infrared spectrometer: antaris II FT-NIR Analyzer Seimer Feishell science, USA, light source; halogen tungsten lamp, detector: InGaAs, integrating sphere diffuse reflection collection system. Resolution 8cm-1Scanning spectral range of 4000-10000 cm-1Number of scans 32 times, room temperature, relative humidity 35%.
The results are shown in the following table, and the absolute deviation between the predicted value and the true value is small, which indicates that the correction model has good prediction capability.
TABLE 2 glycyrrhizic acid content model prediction results
As seen from the table above, in 20 samples of the compound liquorice tablets, the accuracy rate of the glycyrrhizic acid content relative deviation less than 3% reaches 90%, which indicates that the established model has good prediction capability.
(5) Compound licorice tablet sample determination
Introducing the correction model into TQ quantitative analysis software, comprehensively predicting the established correction model in order to improve modeling accuracy, acquiring original spectral data of a new sample of the compound liquorice tablet by using an NIR (near infrared spectroscopy) instrument, inputting the data into the TQ quantitative analysis software introduced with the correction model, and calculating by the software to obtain the index component content, namely a predicted value, of the unknown compound liquorice tablet; and measuring the actual content of the new sample by adopting a corresponding standard method of the high performance liquid chromatography, comparing the predicted value with the true value, and checking the prediction capability of the modeled correction model.
1) Selecting 10 batches of compound liquorice tablet samples to be detected, and acquiring the original spectrum data of the correction set by using a near-infrared spectrometer to obtain the original near-infrared spectrum data of the compound liquorice tablet to be detected. A near-infrared spectrometer: antaris II FT-NIR Analyzer Seimer Feishell science, USA, light source; halogen tungsten lamp, detector: InGaAs, integrating sphere diffuse reflection acquisition system, resolution 8cm-1Scanning spectral range of 4000-10000 cm-1Number of scans 32 times, room temperature, relative humidity 35%.
2) Inputting the collected original near infrared spectrum data into the TQ quantitative analysis software which is introduced into the correction model, and obtaining the content of glycyrrhizic acid through systematic calculation. Meanwhile, the real values of the 10 batches of compound liquorice tablet samples to be detected are measured according to the method in the step (2) and are obtained.
It can also be seen from fig. 3 that the predicted values of the components tested by the model built by the present invention are close to the true values, which indicates that the correction model built by the present invention has good prediction capability.
After repeated experiments and multiple times of verification of the inventor, in the step (1), the calibration set samples can be pretreated under the following conditions: and crushing the correction set compound liquorice tablet sample, sieving the crushed sample with a 50-80-mesh sieve, and drying the sieved part at 60-80 ℃ for 1-5 hours.
Example 2 and example 1 methods for verifying applicability of correction model
This example is to verify the applicability of the calibration model constructed in example 1, and the difference of this example with respect to example 1 is mainly that the object of content measurement in step (5) is glycyrrhiza extract. Specifically, step (5) of this embodiment includes:
collecting original spectral data of a licorice extract sample by using an NIR instrument, inputting the data into TQ quantitative analysis software introduced into a correction model, and calculating by the software to obtain the glycyrrhizic acid content in the licorice extract, namely a predicted value; and performing gradient elution by using octadecylsilane chemically bonded silica as a filler, acetonitrile as a mobile phase A and 0.05% phosphoric acid solution as a mobile phase B by adopting a high performance liquid chromatography, wherein the detection wavelength is 237nm, and the glycyrrhizic acid content, namely the true value, of the licorice extract sample is determined according to a content determination method under the licorice extract item in the first part of pharmacopoeia of the people's republic of China 2015. And comparing the predicted value with the true value, and verifying the applicability of the established correction model.
1) Selecting 10 batches of licorice extract samples to be detected, and acquiring the original spectrum data of the correction set by using a near-infrared spectrometer to obtain the original near-infrared spectrum data of the licorice extract to be detected. A near-infrared spectrometer: antaris II FT-NIR Analyzer Seimer Feishell science, USA, light source; halogen tungsten lamp, detector: InGaAs, integrating sphere diffuse reflection acquisition system, resolution 8cm-1Scanning spectral range of 4000-10000 cm-1Number of scans 32 times, room temperature, relative humidity 35%.
2) Inputting the collected original near infrared spectrum data into the TQ quantitative analysis software which is introduced into the correction model, and obtaining the glycyrrhizic acid content of the 10 batches of extractum glycyrrhizae to be detected through system calculation. Meanwhile, the real values of the 10 batches of the licorice extract samples to be measured are measured according to the content measuring method under the term of the licorice extract in the first part of pharmacopoeia of the people's republic of China 2015 edition, and the real values are obtained.
3) The comparison of the predicted value and the true value of the licorice extract by adopting the experimental example is as follows:
TABLE 3 glycyrrhizic acid content model prediction results
According to the data in the above table, the difference between the predicted value and the true value of glycyrrhizic acid in 10 batches of glycyrrhiza extract samples measured in this example is not large, and the method is also suitable for measuring the effective components of glycyrrhiza extract.
Comparative example 1
This comparative example is a comparative example of example 1, and the difference of this comparative example from example 1 is mainly the difference in establishment of the correction model in step (3). Specifically, step (3) of this comparative example includes:
preprocessing the original spectrum data of the correction set obtained in the step (1) to obtain a glycyrrhizic acid content characteristic spectrum in the compound liquorice tablets; establishing a correction model for glycyrrhizic acid in the compound liquorice tablets, establishing the correction model by using Partial Least Squares (PLS) in TQ quantitative analysis software, and performing external verification by using a verification set sample; the glycyrrhizic acid wave band is selected to be 5600-10000 cm-1The spectral preprocessing method is a first derivative. The rest of the procedure was the same as in example 1. As a result:
(1) the comparison of the predicted value and the true value of the compound liquorice tablets by adopting the comparative example is as follows:
TABLE 4 glycyrrhizic acid content model prediction results
According to the data in the table, the predicted value and the true value of the correction model constructed in the comparative example are greatly different, and the correction model is not suitable for measuring the effective components of the compound liquorice tablets.
(2) The correction model constructed by the comparative example has poor applicability.
TABLE 5 glycyrrhizic acid calibration model parameters established by multivariate Scattering calibration method
| Pretreatment method | Modeling waveband | R2 | RMSEC | | |
| Original spectrum | |||||
| 4000～10000cm-1 | 0.861 | 0.419 | 0.447 | ||
| Example 1 | |
4000～10000cm-1 | 0.979 | 0.179 | 0.197 |
| Comparative example 1 | First derivative of | 5600～10000cm-1 | 0.872 | 0.267 | 0.408 |
According to the results in the table, in the correction model constructed in the comparative example, the RMSEP and the RMSEC are not close and have a large difference, which indicates that the applicability of the constructed model is worse.
Comparative example 2
This comparative example is a comparative example of example 1, and the difference of this comparative example from example 1 is mainly the difference of the sample pretreatment method in step (1). Specifically, step (1) of this comparative example includes:
collecting 80 batches from the compound liquorice tablets, selecting 60 batches as a correction set, selecting 20 batches as a verification set, crushing the samples, sieving the samples with a 60-mesh sieve, and not drying the samples. The rest of the procedure was the same as in example 1. As a result:
(1) the correction model constructed by the comparative example has poor applicability.
TABLE 6 glycyrrhizic acid calibration model parameters established by multivariate Scattering calibration method
| Pretreatment method | Modeling waveband | R2 | RMSEC | | |
| Original spectrum | |||||
| 4000～10000cm-1 | 0.861 | 0.419 | 0.447 | ||
| Example 1 | |
4000～10000cm-1 | 0.979 | 0.179 | 0.197 |
| Comparative example 1 | First derivative of | 5600～10000cm-1 | 0.872 | 0.267 | 0.408 |
| Comparative example 2 | |
4000～10000cm-1 | 0.915 | 0.203 | 0.338 |
According to the results in the table, in the correction model constructed by the comparative example, the RMSEP and the RMSEC are not close to each other and have a large difference, and the constructed model has poor applicability, and the interference of moisture on the detection of the index components can be effectively eliminated by drying the sample.
(2) The comparison of the predicted value and the true value of the compound liquorice tablets by adopting the comparative example is as follows:
TABLE 7 glycyrrhizic acid content model prediction results
According to the data in the table, the predicted value and the true value of the correction model constructed in the comparative example are greatly different, the correction model is not suitable for measuring the effective components of the compound liquorice tablets, and the prediction capability of the content correction model is low.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A construction method of a model for measuring the content of active ingredients of compound liquorice tablets is characterized by comprising the following steps:
(1) taking a plurality of compound liquorice tablet samples as a correction set, and scanning by near infrared light to obtain original spectral data of the correction set;
(2) performing spectrum preprocessing on the original spectrum data of the correction set, selecting a modeling waveband of the effective component, and acquiring a content characteristic spectrum of the effective component;
(3) respectively measuring the effective components of the multiple compound liquorice tablet samples contained in the correction set by adopting a high performance liquid chromatography to obtain the true content values of the effective components;
(4) correlating the content characteristic spectrum obtained in the step (2) and the content true value obtained in the step (3) by using a partial least square method, and establishing a content correction model of the effective component; the effective component is glycyrrhizic acid.
2. The method for constructing a model for measuring the content of active ingredients in compound liquorice tablets according to claim 1, wherein the step (1) comprises the following pretreatment of a calibration set and then near-infrared light scanning: and crushing the correction set compound liquorice tablet sample, sieving the crushed sample with a 50-80-mesh sieve, and drying the sieved part at 60-80 ℃ for 1-5 hours.
3. The method for constructing a model for measuring the content of active ingredients in compound licorice tablets according to claim 1, wherein in the step (2), the spectrum pretreatment method is multivariate scattering correction, and the modeling waveband is 4000-10000 cm-1The number of main factors is 7-10.
4. The method for constructing a model for measuring the content of active ingredients in compound licorice tablets according to claim 3, wherein in the step (2), the spectrum pretreatment method is multivariate scattering correction, and the modeling waveband is 4000-10000 cm-1The number of main factors is 10.
5. The method for constructing a model for measuring the content of active ingredients in compound licorice tablets according to any one of claims 1 to 4, wherein the method comprises: taking a plurality of compound liquorice tablet samples as a verification set, preprocessing the samples, and scanning the samples by near infrared light to obtain original spectral data of the verification set; and importing the original spectrum data of the verification set into the original spectrum data of the verification set for verification.
6. The method for constructing a model for measuring the content of active ingredients in FUFANGGANCAO tablet according to any one of claims 1 to 4, wherein the near infrared light scanning conditions include: resolutionThe rate is 3-10 cm-1Scanning spectral range of 4000-10000 cm-1The scanning times are 30-35 times, the temperature is 22-28 ℃, and the relative humidity is 32-38%.
7. The method for constructing a model for measuring the content of active ingredients in compound liquorice tablets according to claim 6, wherein the near-infrared light scanning conditions comprise: resolution 8cm-1Scanning spectral range of 4000-10000 cm-1The number of scans was 32, 25 ℃ and relative humidity 35%.
8. A detection method for the content of active ingredients of compound liquorice tablets is characterized by comprising the following steps:
taking a compound liquorice tablet sample to be detected, and scanning by near infrared light to obtain original spectral data of the compound liquorice tablet sample to be detected;
inputting the original spectral data of the compound liquorice tablet sample to be detected into a chemometric analysis system introduced with a content correction model constructed according to any one of claims 1 to 7, and obtaining the content of the effective components of the compound liquorice tablet sample to be detected through calculation; the effective component is glycyrrhizic acid.
9. The method for detecting the content of the active ingredients in the compound liquorice tablets as claimed in claim 8, wherein the compound liquorice tablet to be detected is crushed and sieved by a 50-80-mesh sieve, and then the sieved part is dried at 60-80 ℃ for 1-5 hours.
10. The method for detecting the content of the active ingredients in the compound liquorice tablets according to claim 8 or 9, wherein the near-infrared light scanning conditions comprise: resolution ratio of 3-10 cm-1Scanning spectral range of 4000-10000 cm-1The scanning times are 30-35 times, the temperature is 22-28 ℃, and the relative humidity is 32-38%.
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