CN110308108A - Content of baicalin detection method and system based on terahertz time-domain spectroscopic technology - Google Patents
Content of baicalin detection method and system based on terahertz time-domain spectroscopic technology Download PDFInfo
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- CN110308108A CN110308108A CN201910635190.7A CN201910635190A CN110308108A CN 110308108 A CN110308108 A CN 110308108A CN 201910635190 A CN201910635190 A CN 201910635190A CN 110308108 A CN110308108 A CN 110308108A
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- IPQKDIRUZHOIOM-UHFFFAOYSA-N Oroxin A Natural products OC1C(O)C(O)C(CO)OC1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 IPQKDIRUZHOIOM-UHFFFAOYSA-N 0.000 title claims abstract description 54
- IKIIZLYTISPENI-ZFORQUDYSA-N baicalin Chemical compound O1[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 IKIIZLYTISPENI-ZFORQUDYSA-N 0.000 title claims abstract description 54
- 229960003321 baicalin Drugs 0.000 title claims abstract description 54
- AQHDANHUMGXSJZ-UHFFFAOYSA-N baicalin Natural products OC1C(O)C(C(O)CO)OC1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 AQHDANHUMGXSJZ-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000001514 detection method Methods 0.000 title claims abstract description 34
- 238000005516 engineering process Methods 0.000 title claims abstract description 25
- 239000000203 mixture Substances 0.000 claims abstract description 49
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- XDQITMCFPPPMBC-TUANDBMESA-N scutelloside Natural products OC[C@H]1O[C@@H](O[C@@H]2O[C@@H]3C[C@H]4[C@H](O)[C@@H](O)[C@@](O)(CO3)[C@@H]24)[C@H](O)[C@@H](O)[C@@H]1O XDQITMCFPPPMBC-TUANDBMESA-N 0.000 claims abstract description 22
- 238000010521 absorption reaction Methods 0.000 claims abstract description 12
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- 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
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- 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
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- G—PHYSICS
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- 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
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- 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
- G01N21/3581—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using far infrared light; using Terahertz radiation
- G01N21/3586—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using far infrared light; using Terahertz radiation by Terahertz time domain spectroscopy [THz-TDS]
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- 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
- G01N2021/3196—Correlating located peaks in spectrum with reference data, e.g. fingerprint data
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- 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
- G01N2021/3572—Preparation of samples, e.g. salt matrices
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- 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
- G01N2021/3595—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR
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Abstract
Present disclose provides a kind of content of baicalin detection method and system based on terahertz time-domain spectroscopic technology, prepare the sample of the different mixture of content of baicalin;The unloaded terahertz time-domain signal with sample of acquisition;The terahertz time-domain signal of zero load and sample to acquisition carries out Fourier transformation, obtains with reference to the Terahertz frequency-region signal with sample, calculates the terahertz absorption spectra for obtaining mixture.The absorption data of spectrum are pre-processed, the similarity of the mixture absorption spectra of each proportion is calculated, rejecting abnormalities spectrum divides sample, is divided into calibration set and verifying collection;Using the Terahertz absorption spectra of calibration set and corresponding Determination of baicalin information as input, the content of baicalin prediction model based on calibration set sample data is established with Partial Least Squares, prediction model is verified, satisfactory prediction model is verified in output;Scutelloside sample to be detected is detected using the prediction model, output test result.
Description
Technical field
The disclosure belongs to spectral detection field, and in particular to a kind of scutelloside based on terahertz time-domain spectroscopic technology contains
Quantity measuring method and system.
Background technique
Only there is provided background technical informations relevant to the disclosure for the statement of this part, it is not necessary to so constitute first skill
Art.
It is drug quality inspection in the ingredient identification and the measurement of content of active component of the field of medicament such as medicine production, supervision
The key content of survey.Scutelloside (Baicalin) is that a kind of flavone compound separated is extracted from scutellariae,radix, is had
Significant bioactivity has antibacterial, diuresis, anti-inflammatory, resistance state and spasmolysis, and with stronger antitumor response etc.
Physiological potency occupies an important position in clinical medicine.Scutelloside is the effective component of many common Chinese patent drugs, such as silver yellow
Particle, Qingkailing granule, flu cough-stopping granule, Xiao Chai Hu granules etc., content influence drug effect, the physicochemical property of drug
It is great, it is the major quality controlling index of radix scutellariae and its preparation.
Currently, drug ingedient analysis method mainly includes high performance liquid chromatography (HPLC) method, infrared spectroscopy, ultraviolet spectra
Method etc..HPLC is that the defined liquid dissolved with measured matter is input to the chromatography equipped with filler using high pressure transfusion system
In column, to realize the separation determination to substance, HPLC method efficiency is high and adaptable, it require that standard in advance
Standby sample, sample treatment is relatively complicated, analysis time is longer and reagent cost is higher.Infrared spectroscopy is to answer in recent years
With a kind of relatively broad analysis method, it passes through analysis of the effect to realization to substance between measurement of species and spectrum,
This method analysis speed is fast, and to sample without chemical contamination, instrumentation is simple, is also applied to the detection of many drugs at present
In.Ultraviolet spectra is also a kind of common substance spectra detection means, but ultraviolet spectra is chiefly used in the very low liquid of analytical concentration
Body sample, the work quickly analyzed using it solid sample is still rare, therefore the popularization in drug test also receives
Certain limitation.
Summary of the invention
The disclosure to solve the above-mentioned problems, proposes a kind of content of baicalin based on terahertz time-domain spectroscopic technology
Detection method and system, the disclosure utilize strong penetrability, dactylogram and the collective to reaction molecular configuration and conformation of Terahertz
Vibration has the characteristic of very strong sensitivity, establishes the prediction model of content of baicalin, and evaluated model, verified, and realizes
Fast and accurate prediction to content of baicalin.
According to some embodiments, the disclosure is adopted the following technical scheme that
A kind of content of baicalin detection method based on terahertz time-domain spectroscopic technology, comprising the following steps:
Prepare the sample of the different mixture of content of baicalin;
The unloaded terahertz time-domain signal with sample of acquisition;
The terahertz time-domain signal of zero load and sample to acquisition carries out Fourier transformation, obtains reference and sample too
Hertz frequency-region signal, calculates the terahertz absorption spectra for obtaining mixture.
The absorption data of spectrum are pre-processed, the similarity of the mixture absorption spectra of each proportion is calculated, are rejected
Exceptional spectrum divides sample, is divided into calibration set and verifying collection;
Using the Terahertz absorption spectra of calibration set and corresponding Determination of baicalin information as input, with Partial Least Squares
The content of baicalin prediction model based on calibration set sample data is established, prediction model is evaluated and is verified.
Scutelloside sample to be detected is detected using the prediction model, output test result.
As possible embodiment, the sample of mixture at least containing scutelloside and other a kind of or more substances,
Tabletting and drying are carried out to mixture.
As possible embodiment, acquired using the transmission mode of terahertz time-domain spectroscopy system unloaded and sample
Terahertz time-domain signal.
As possible embodiment, the terahertz time-domain spectroscopy system includes laser, beam splitter, delay line, light
Conductance antenna, paraboloidal mirror, lens, reflecting mirror, tin indium oxide pellicle, electro-optic crystal, quarter wave plate, Wollaston rib
The laser of mirror, balanced type photodetector, lock-in amplifier and displacement platform, laser transmitting is divided into detection by beam splitter
Light and pump light, the detection light form the first light beam after delay line and reflecting mirror;The pump light shines by optical path
It is mapped on photoconductive antenna and generates terahertz emission, terahertz emission is radiated on sample after paraboloidal mirror, lens, warp
The light of sample is crossed after another lens and paraboloidal mirror, forms the second light beam, it is thin that two light beams enter tin indium oxide light splitting
Film successively after electro-optic crystal, lens, quarter wave plate, Wollaston prism, balanced type photodetector and lock-in amplifier,
Signal is transferred to computer, and institute's translation stage drives sample to carry out two dimensional motion.
As possible embodiment, is obtained by Fourier transformation with reference to the Terahertz frequency-region signal with sample, calculated
Obtain the terahertz absorption spectra of mixture.
As possible embodiment, the pretreatment is to be filtered to absorption data.
As possible embodiment, the similarity of the mixture absorption spectra of each proportion is calculated using mahalanobis distance,
Rejecting abnormalities spectrum.
As possible embodiment, the sample of selection is divided into calibration set and verifying collects, the mixing of each proportion
Object in the same proportion, while the sample number of calibration set be greater than verifying collection sample number.
As possible embodiment, using the Terahertz absorption spectra of calibration set and corresponding Determination of baicalin information as
Input establishes the content of baicalin prediction model based on calibration set sample data with Partial Least Squares;
The content of baicalin prediction model established using the sample data inspection institute of verifying collection, by calculating related coefficient
With the reliability and precision of root-mean-square error evaluation model, if related coefficient and root-mean-square error meet setting range, model
It meets the requirements.
A kind of content of baicalin detection system based on terahertz time-domain spectroscopic technology, comprising:
Acquire the terahertz time-domain signal of the zero load of terahertz time-domain spectroscopy system and the sample of mixture;
The terahertz time-domain signal of zero load and sample to acquisition carries out Fourier transformation, obtains reference and sample too
Hertz frequency-region signal, calculates the terahertz absorption spectra for obtaining mixture;
It according to processing module, is configured as the absorption data to spectrum and pre-processes, calculate the mixture of each proportion
The similarity of absorption spectra, rejecting abnormalities spectrum, divides sample, is divided into calibration set and verifying collection;
Model construction module is configured as making the Terahertz absorption spectra of calibration set and corresponding Determination of baicalin information
For input, with Partial Least Squares establish the content of baicalin prediction model based on calibration set sample data, to prediction model into
Row evaluation and verifying;
Detection module is configured as detecting scutelloside sample to be detected using the prediction model, output inspection
Survey result.
Compared with prior art, the disclosure has the beneficial effect that
The disclosure using the strong penetrability of Terahertz, dactylogram and has the collective vibration of reaction molecular configuration and conformation
The characteristic of very strong sensitivity establishes the prediction model of content of baicalin, and is evaluated model, verified, and realizes to radix scutellariae
The fast and accurate prediction of glycosides content;It for non-contact detection, does not need to carry out pre-processing to sample, does not have to destroy to be measured
Sample, be it is a kind of efficiently, fast and accurately detection method.In addition, terahertz emission does not ionize injury, safety to human body
It is high.
Detailed description of the invention
The Figure of description for constituting a part of this disclosure is used to provide further understanding of the disclosure, the disclosure
Illustrative embodiments and their description do not constitute the improper restriction to the disclosure for explaining the disclosure.
Fig. 1 is transmission-type terahertz time-domain spectroscopy system principle schematic diagram.
Fig. 2 is the terahertz absorption spectra of various concentration scutelloside mixture.
Fig. 3 is the terahertz absorption spectra of scutelloside, sucrose and cornstarch.
Fig. 4 relationship between calibration set Determination of baicalin predicted value and actual value.
Fig. 5 is relationship between verifying collection Determination of baicalin predicted value and actual value.
Specific embodiment:
The disclosure is described further with embodiment with reference to the accompanying drawing.
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the disclosure.Unless
Otherwise indicated, all technical and scientific terms used herein has and disclosure person of an ordinary skill in the technical field
Normally understood identical meanings.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to the illustrative embodiments of the disclosure.As used herein, unless the context clearly indicates otherwise, otherwise singular shape
Formula be also intended to include plural form, additionally, it should be understood that, when in the present specification use term "comprising" and/or
When " comprising ", existing characteristics, step, operation, device, component and/or their combination are indicated.
A method of based on terahertz time-domain spectroscopic technology quick predict content of baicalin comprising the steps of:
(1) sample is prepared:
It prepares the different mixture of content of baicalin and carries out the sample of terahertz light spectrometry.Mixture by scutelloside,
Three kinds of sucrose and cornstarch at being grouped as, can also by other it is two kinds or more of containing scutelloside at being grouped as.It will mixing
Object tablet press machine is pressed into the parallel thin slice in surface.Before test, it by sample drying, excludes water in sample and experiment is tied
The influence of fruit.
(2) terahertz absorption spectra acquires
The relative humidity for testing environment is reduced to 3% hereinafter, adopting using the transmission mode of terahertz time-domain spectroscopy system
The unloaded terahertz time-domain signal with sample of collection.It is obtained by Fourier transformation with reference to the Terahertz frequency-region signal with sample, warp
It crosses optics formula and calculates the terahertz absorption spectra for obtaining mixture;Calculation formula:
Wherein, A is absorption spectra data, EsamAnd ErefIt is divided into sample frequency domain data and with reference to frequency domain data, d is sample
Thickness.
(3) pretreatment of spectrum
Using Savitzky-Golay filter to absorb data pre-process, the high-frequency noise of lowering apparatus and its
His random noise, smooth absorption spectrum curve and undistorted absorption waveform and absorption characteristic.
(4) samples selection
The similarity of the mixture absorption spectra of each proportion, rejecting abnormalities spectrum are calculated using mahalanobis distance.
(5) sample divides
The sample of selection is divided into calibration set and verifying collection;The sample ratio of calibration set and verifying collection is according to 2:1 or 3:
1 or 4:1 is divided, and the mixture of each proportion is in the same proportion;The sample number of calibration set is greater than the sample number of verifying collection;
(6) foundation of content of baicalin prediction model
Using the Terahertz absorption spectra of calibration set and corresponding Determination of baicalin information as input, with Partial Least Squares
Establish the content of baicalin prediction model based on calibration set sample data;
(7) verifying of model
Utilize the performance for the content of baicalin prediction model that the sample data checking procedure (6) of verifying collection is established.
(8) evaluation of model
By the reliability and precision that calculate related coefficient and root-mean-square error evaluation model;Related coefficient closer to
1, root-mean-square error is smaller, and model accuracy is higher.
The frequency range of Terahertz be 0.1~10THz, in electromagnetic spectrum between microwave and infra-red radiation.Terahertz
Hereby radiation has low energy, wide spectrum and the feature penetrated by force, and ionization will not be caused to destroy to substance, and Terahertz absorbs
Spectrum absorption peak is obvious, overlapping is few, has fingerprint characteristic.Therefore, terahertz time-domain spectroscopic technology has many transmission spectra technologies
The advantages of do not had, is the emerging non-destructive testing technology of great competitiveness developed in recent years, is gradually applied to cure
It treats, chemicals analysis, food quality controls and the fields such as non-destructive testing.In addition, tera-hertz spectra can be weak between reaction molecular
Active force all has very strong sensitivity to the fine difference of collective vibration mode and space structure, these good characteristics make
Terahertz light spectral technology can be applied to that the structure of matter, physical property are analyzed and identified, produce in Chinese traditional medicinal materials recognition, Chinese medicine
Its potentiality is gradually shown in the drugs Quality Detection related fieldss such as ground identifies, Chinese medicine composition is analyzed and component quantifying measures
And advantage.The present embodiment is based on terahertz time-domain spectroscopic technology combination stoechiometric process Partial Least Squares and detects mixture
The content of middle scutelloside.
The content of special component influences drug effect, the physicochemical property of drug great in drug, therefore to certain ingredients
Quantitative detection is extremely important.It is lossless, accurately and rapidly detection method be realize quality assurance, real-time detection important prerequisite.
As the development of Chemical Measurement and applicability enhance, Partial Least Squares (PLS) be widely used in spectrum analysis and at
In the quantitative detection divided.Partial Least Squares has concentrated principal component analysis, canonical correlation analysis and multiple linear regression analysis three
The advantages of kind analysis method, can not only provide more reasonable regression model in analysis result, can also be completed at the same time
The research contents of principal component analysis and canonical correlation analysis provides richer, deep information.
The present embodiment uses terahertz time-domain spectroscopy system FiCO, generates and the method for detection Terahertz is respectively photoelectricity
Lead antenna and electro optic sampling, the available frequency range of the system are 0-3THz.System is mainly by femto-second laser, time delay
System, terahertz sources head and Terahertz receive head composition.Attached drawing 1 is the schematic illustration under the system transmittance operating mode.
Embodiment 1: please referring to shown in Fig. 1 to Fig. 5, utilizes terahertz time-domain spectroscopic technology knot the present embodiment provides a kind of
The method for closing Partial Least Squares detection content of baicalin, comprising the following steps:
(1) sample prepares:
The purity of scutelloside is 98%, and sucrose and cornstarch are excipient substance grade;Scutelloside and sucrose and corn are formed sediment
It is 3%, 5%, 10%, 20%, 30%, 40% that powder, which is configured to content of baicalin according to weight, and 50% waits the mixing of 7 concentration
The ratio of object, each mixture sucrose and cornstarch is 4:1, the different mixture of simulation content of baicalin.Mixture is put
It is placed on oscillator and vibrates, be sufficiently mixed mixture uniformly.The mixture that quality is 0.2g/ parts is pressed into 10MPa pressure
The parallel thin rounded flakes in surface, thickness are about 1mm, diameter 13mm.The mixture and scutelloside of each concentration, sucrose and
Each tabletting of the pure substance of cornstarch 10, totally 100 samples, before test, sample is placed in 40 DEG C of vacuum drying
Case is 12 hours dry, excludes influence of the water to experimental result in sample.
(2) experiment test prepares: in order to avoid the influence of water vapor in air, terahertz time-domain spectroscopy system being placed
In seal closure, and dry air is filled into seal closure, the air humidity of seal closure is controlled below 3%.
(3) it obtains time-domain signal: in a transmissive mode, sample being placed in sample slot, to terahertz time-domain spectroscopy system
After system booting is stablized, when test is unloaded and it is loaded the time-domain signal of this when, respectively as reference signal and sample signal.
(4) time frequency signal converts: reference signal and the time domain waveform of sample signal being carried out Fourier transformation, joined
Examine the frequency-domain waveform E of signal and sample signalrefAnd Esam。
(5) Application Optics formula calculates the terahertz absorption spectra for obtaining mixture, calculation formula:
Wherein, A is absorption spectra data, EsamAnd ErefIt is divided into sample frequency domain data and with reference to frequency domain data, d is sample
Thickness.Since terahertz emission passes through the decaying of sample, selecting spectrum according to the signal-to-noise ratio of signal can be 0.3- with section
1.5THz。
(6) using Savitzky-Golay filter to absorb data pre-process, the high-frequency noise of lowering apparatus and
Other random noises, smooth absorption spectrum curve and undistorted absorption waveform and absorption characteristic.
(7) print of every kind of mixture is 10, and 2 points of each prototype test, every kind of mixture has 20 absorption spectra numbers
According to, altogether obtain 140 absorption spectra datas.Using mahalanobis distance method rejecting abnormalities spectrum, each mixture is calculated by mahalanobis distance
The similarity of absorption spectra, every kind of mixture selection press 3%, 5%, 10%, 20% apart from the smallest preceding 15 spectrum,
30%, 40%, 50% concentration sequence number consecutively selects 105 samples altogether.Mixture and scutelloside, sucrose and the shallow lake measured
The tera-hertz spectra of powder pure substance, spectrum are as shown in Figures 2 and 3.
(8) 105 samples are divided into two groups to be calibrated and verified respectively, verifying collection is used to assess calibration set foundation
The accuracy of model.Using 70 samples as calibration set, 35 samples is used to collect as verifying, the mixture of each proportion
It is all identical that calibration set and verifying collect contained sample proportion.
(9) using the Terahertz absorption spectra of calibration set and corresponding Determination of baicalin information as input, utilization minimum two partially
Multiplication establishes the concentration of scutelloside in mixture and absorbs the model between response, and the frequency range for inputting absorption spectrum is
0.3-1.5THz, the relationship between calibration set Determination of baicalin predicted value and actual value are as shown in Fig. 5.
(10) scutelloside established using the Terahertz absorption spectra and corresponding Determination of baicalin information inspection institute of verifying collection
The performance of content prediction model, the relationship between verifying collection Determination of baicalin predicted value and actual value are as shown in Fig. 5.
(11) pass through the reliability and precision of calculating related coefficient (R) and root-mean-square error (RMSE) evaluation model.It is related
The variance var (y) of the variance var (x) and y of the covariance cov (x, y) of coefficient and variable x and variable y, x are related, R=cov
(x,y)/(var(x)*var(y))1/2, the calculation method of RMSE is RMSE=(∑ (x-y)2/n)1/2, n is sample number, x and y
Respectively represent actual concentrations and prediction concentrations.The value of R is smaller closer to 1, RMSE, shows that the precision of the model is higher.Experiment
In, the R value of calibration set is 0.9982, RMSE 1.41%, it was demonstrated that the validity of calibrating patterns.Meanwhile verify collection R and
RMSE is respectively 0.9972 and 1.26%.Two groups of high R and small RMSE show that prediction data is very close with actual value, calibrating die
Type is also quite correct.
Therefore, terahertz time-domain spectroscopic technology combination Partial Least Squares is to the quantitative determination of scutelloside in mixture
Reliably, it can be quantitative determined within the scope of Terahertz according to absorption spectra data using Partial Least Squares yellow in mixture
The concentration of a kind of reed mentioned in ancient books glycosides.
It should be understood by those skilled in the art that, embodiment of the disclosure can provide as method, system or computer journey
Sequence product.Therefore, complete hardware embodiment, complete software embodiment or combining software and hardware aspects can be used in the disclosure
The form of embodiment.Moreover, it wherein includes the calculating of computer usable program code that the disclosure, which can be used in one or more,
The computer program implemented in machine usable storage medium (including but not limited to magnetic disk storage, CD-ROM, optical memory etc.)
The form of product.
The disclosure is referring to method, the process of equipment (system) and computer program product according to the embodiment of the present disclosure
Figure and/or block diagram describe.It should be understood that can be realized by computer program instructions each in flowchart and/or the block diagram
The combination of process and/or box in process and/or box and flowchart and/or the block diagram.It can provide these computers
Processor of the program instruction to general purpose computer, special purpose computer, Embedded Processor or other programmable data processing devices
To generate a machine, so that being generated by the instruction that computer or the processor of other programmable data processing devices execute
For realizing the function of being specified in one or more flows of the flowchart and/or one or more blocks of the block diagram
Device.
These computer program instructions, which may also be stored in, is able to guide computer or other programmable data processing devices with spy
Determine in the computer-readable memory that mode works, so that instruction stored in the computer readable memory generation includes
The manufacture of command device, the command device are realized in one box of one or more flows of the flowchart and/or block diagram
Or the function of being specified in multiple boxes.
These computer program instructions also can be loaded onto a computer or other programmable data processing device, so that
Series of operation steps are executed on computer or other programmable devices to generate computer implemented processing, thus calculating
The instruction executed on machine or other programmable devices is provided for realizing in one or more flows of the flowchart and/or side
The step of function of being specified in block diagram one box or multiple boxes.
The foregoing is merely preferred embodiment of the present disclosure, are not limited to the disclosure, for the skill of this field
For art personnel, the disclosure can have various modifications and variations.It is all the disclosure spirit and principle within, it is made any
Modification, equivalent replacement, improvement etc., should be included within the protection scope of the disclosure.
Although above-mentioned be described in conjunction with specific embodiment of the attached drawing to the disclosure, not the disclosure is protected
The limitation of range, those skilled in the art should understand that, on the basis of the technical solution of the disclosure, those skilled in the art
Member does not need to make the creative labor the various modifications or changes that can be made still within the protection scope of the disclosure.
Claims (10)
1. a kind of content of baicalin detection method based on terahertz time-domain spectroscopic technology, it is characterized in that: the following steps are included:
Prepare the sample of the different mixture of content of baicalin;
The unloaded terahertz time-domain signal with sample of acquisition;
The terahertz time-domain signal of zero load and sample to acquisition carries out Fourier transformation, obtains with reference to the Terahertz frequency with sample
Domain signal calculates the terahertz absorption spectra for obtaining mixture;
The absorption data of spectrum are pre-processed, the similarity of the mixture absorption spectra of each proportion, rejecting abnormalities are calculated
Spectrum divides sample, is divided into calibration set and verifying collection;
Using the Terahertz absorption spectra of calibration set and corresponding Determination of baicalin information as input, base is established with Partial Least Squares
In the content of baicalin prediction model of calibration set sample data, prediction model is evaluated and is verified, output verifying conforms to
The prediction model asked;
Scutelloside sample to be detected is detected using the prediction model, output test result.
2. a kind of content of baicalin detection method based on terahertz time-domain spectroscopic technology as described in claim 1, feature
Be: the sample of mixture at least containing scutelloside and other a kind of or more substances, carries out tabletting and drying to mixture.
3. a kind of content of baicalin detection method based on terahertz time-domain spectroscopic technology as described in claim 1, feature
It is: acquires unloaded and sample terahertz time-domain signal using the transmission mode of terahertz time-domain spectroscopy system.
4. a kind of content of baicalin detection method based on terahertz time-domain spectroscopic technology as claimed in claim 3, feature
Be: the terahertz time-domain spectroscopy system includes laser, beam splitter, delay line, photoconductive antenna, paraboloidal mirror, lens, anti-
Penetrate mirror, tin indium oxide pellicle, electro-optic crystal, quarter wave plate, Wollaston prism, balanced type photodetector, locking phase amplification
The laser of device and displacement platform, laser transmitting is divided into detection light and pump light by beam splitter, and the detection light is by delay
After line and reflecting mirror, the first light beam is formed;The pump light is irradiated on photoconductive antenna by optical path and generates terahertz emission,
Terahertz emission is radiated on sample after paraboloidal mirror, lens, passes through another lens and paraboloidal mirror by the light of sample
Afterwards, formed the second light beam, two light beams enter tin indium oxide pellicle successively pass through electro-optic crystal, lens, quarter wave plate,
After Wollaston prism, balanced type photodetector and lock-in amplifier, signal is transferred to computer, and institute's translation stage drives
Sample carries out two dimensional motion.
5. a kind of content of baicalin detection method based on terahertz time-domain spectroscopic technology as described in claim 1, feature
It is: is obtained by Fourier transformation with reference to the Terahertz frequency-region signal with sample, the Terahertz that calculating obtains mixture absorbs light
Spectrum.
6. a kind of content of baicalin detection method based on terahertz time-domain spectroscopic technology as described in claim 1, feature
Be: the pretreatment is to be filtered to absorption data.
7. a kind of content of baicalin detection method based on terahertz time-domain spectroscopic technology as described in claim 1, feature
It is: calculates the similarity of the mixture absorption spectra of each proportion, rejecting abnormalities spectrum using mahalanobis distance.
8. a kind of content of baicalin detection method based on terahertz time-domain spectroscopic technology as described in claim 1, feature
Be: the sample of selection being divided into calibration set and verifying collects, the mixture of each proportion in the same proportion, while calibration set
Sample number be greater than verifying collection sample number.
9. a kind of content of baicalin detection method based on terahertz time-domain spectroscopic technology as described in claim 1, feature
It is: using the Terahertz absorption spectra of calibration set and corresponding Determination of baicalin information as input, base is established with Partial Least Squares
In the content of baicalin prediction model of calibration set sample data;
Or, using verifying collection sample data inspection institute establish content of baicalin prediction model, by calculate related coefficient and
The reliability and precision of root-mean-square error evaluation model, if related coefficient and root-mean-square error meet setting range, model symbol
It closes and requires.
10. a kind of content of baicalin detection system based on terahertz time-domain spectroscopic technology, it is characterized in that: including:
Acquire the terahertz time-domain signal of the zero load of terahertz time-domain spectroscopy system and the sample of mixture;
Data processing module, the terahertz time-domain signal for being configured as the zero load and sample to acquisition carry out Fourier transformation, obtain
It obtains with reference to the Terahertz frequency-region signal with sample, calculates the terahertz absorption spectra for obtaining mixture.To the absorption data of spectrum
It being pre-processed, calculates the similarity of the mixture absorption spectra of each proportion, rejecting abnormalities spectrum divides sample,
It is divided into calibration set and verifying collection;
Model construction module is configured as using the Terahertz absorption spectra of calibration set and corresponding Determination of baicalin information as defeated
Enter, the content of baicalin prediction model based on calibration set sample data is established with Partial Least Squares, prediction model is commented
Valence and verifying;
Detection module is configured as detecting scutelloside sample to be detected using the prediction model, output detection knot
Fruit.
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