CN106404711A - A method of discriminating common yam rhizome wall-broken decoction piece adulteration - Google Patents
A method of discriminating common yam rhizome wall-broken decoction piece adulteration Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 47
- 244000281702 Dioscorea villosa Species 0.000 title abstract 6
- 229920002472 Starch Polymers 0.000 claims abstract description 60
- 238000002329 infrared spectrum Methods 0.000 claims abstract description 37
- 229920002261 Corn starch Polymers 0.000 claims abstract description 17
- 238000004458 analytical method Methods 0.000 claims abstract description 17
- 239000008120 corn starch Substances 0.000 claims abstract description 17
- 230000008569 process Effects 0.000 claims abstract description 14
- 239000003814 drug Substances 0.000 claims description 141
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- 229940099112 cornstarch Drugs 0.000 claims description 16
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 235000019425 dextrin Nutrition 0.000 claims description 7
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 7
- 239000001863 hydroxypropyl cellulose Substances 0.000 claims description 7
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- 239000008101 lactose Substances 0.000 claims description 7
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- 229940016286 microcrystalline cellulose Drugs 0.000 claims description 7
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- 229910002027 silica gel Inorganic materials 0.000 claims description 7
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- 238000004611 spectroscopical analysis Methods 0.000 claims description 6
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- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 claims description 4
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- 244000096857 Dioscorea batatas Species 0.000 description 1
- 241000234272 Dioscoreaceae Species 0.000 description 1
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- 241000209140 Triticum Species 0.000 description 1
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- 235000004879 dioscorea Nutrition 0.000 description 1
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- 238000004128 high performance liquid chromatography Methods 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
- G01N21/31—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
A method of discriminating common yam rhizome wall-broken decoction piece adulteration is disclosed. The method adopts a near infrared spectrum process and a stoichiometry process to build qualitative and quantitative models of adulterated common yam rhizome wall-broken decoction piece samples doped with corn starch or wheat starch and auxiliary-material-added common yam rhizome wall-broken decoction piece samples. Near infrared spectrum data of a common yam rhizome wall-broken decoction piece sample to be detected is substituted into the models for discrimination, thus acquiring a discriminating result of the sample to be detected. The method can directly perform qualitative and quantitative analysis on common yam rhizome wall-broken decoction piece adulteration, avoids tedious pretreatment steps, has advantages of simple and convenient operation, short analysis time, no damage to samples, environment protection, and the like which are incomparable by conventional analytic methods, greatly shortens the analysis period and reduces an experiment cost.
Description
Technical field
The present invention relates to tcm product quality monitoring field, in particular it relates to a kind of discriminating Chinese yam broken wall medicine materical crude slice is adulterated
Method.
Background technology
Chinese yam（Shanyao）, this product is Dioscoreaceae plant Chinese yamDioscorea oppositaThunb. dry root
Stem.Winter cauline leaf is excavated after withering, and cuts root head, cleans, and removes crust and fibrous root, is dried.Or take advantage of fresh-cut sheet, it is dried,
Have select loose straight Chinese yam is dried, put in clear water, be dipped into the no dry heart, vexed, trim two ends, be twisted into plank cylindric,
Dry, polishing, practise and claim " light yam ".
Chinese medicine wall cell disruption medicine materical crude slice is using modern superfine communication technique, traditional medicine materical crude slice to be carried out breaking cell wall to be ground into size distribution D90
Less than the subparticle of 45um, then the particle making 30-100 mesh.There is color and luster unanimously with respect to traditional medicine materical crude slice, quality is homogeneous,
The feature of good stability is the innovative prepared slices of Chinese crude drugs.In recent years, broken wall medicine materical crude slice innovates category as the prepared slices of Chinese crude drugs, by its promotion
The unique advantages such as Effective Component of Chinese Medicine more preferably absorbs and carries, taking convenience, enjoy consumers in general to favor, in traditional Chinese medicine and guarantor
Health food market portion continues to increase, economic worth is growing.
Chinese yam broken wall medicine materical crude slice is a kind of product being used as medicine without any additive or pharmaceutic adjuvant, full composition, Chinese yam by
At a relatively high with medical value in idiotrophic, widely consumer accept, some illegal enterprises in order to obtain illegitimate benefits, on mountain
Mix in medicine cheap corn, wheaten starch or auxiliary material make particle forge Chinese yam broken wall medicine materical crude slice sold, this illegal row
The market order for not only heavy damage, causes consumer's economic loss, and is unfavorable for that consumer's is healthy.And for
Add the illegal Chinese yam broken wall medicine materical crude slice that other pharmaceutic adjuvants or wheat and corn starch are made, from being difficult in appearance distinguish.Therefore, grind
Study carefully a kind of quick, accurate, stable method qualitative and quantitative detection illegal additive of Chinese yam broken wall medicine materical crude slice of exploitation and seem particularly heavy
Will.
At present, it is not yet found that closing broken wall medicine materical crude slice or similar medicine materical crude slice（Ultramicro-powder etc.）Adulterated authentication technique method.Existing normal
The analytical technologies such as the high performance liquid chromatography of rule, chromatograph-mass spectrometer coupling, microscopical characters, Electronic Nose, DNA molecular identification are required to numerous
Trivial sample pretreatment process, wastes time and energy, and operating personnel's specialized capability is required higher, and experimentation can be to sample or ring
Border pollutes, and testing cost is high.
Content of the invention
The present invention, in order to overcome the above-mentioned deficiency of prior art, provides a kind of model differentiating that Chinese yam broken wall medicine materical crude slice is adulterated.
It is a further object to provide a kind of method differentiating that Chinese yam broken wall medicine materical crude slice is adulterated.
To achieve these goals, the present invention is achieved by the following technical programs：
A kind of model differentiating that Chinese yam broken wall medicine materical crude slice is adulterated, method for building up is as follows：
（1）Starch adulterated Chinese yam broken wall medicine materical crude slice qualitative model is set up：Gather pure Chinese yam broken wall medicine materical crude slice sample, adulterated Chinese yam broken wall
The near infrared spectrum data of medicine materical crude slice sample, data is divided into calibration set and forecast set；Light harvesting modal data will be corrected import
SIMCA-P 12.0 software carries out first derivative/MSC pretreatment, sets up OPLS-DA qualitative model；Described starch forms sediment for corn
One of powder, wheaten starch or tapioca or any combination；
（2）Add auxiliary material Chinese yam broken wall medicine materical crude slice qualitative model to set up：Gather pure Chinese yam broken wall medicine materical crude slice sample, add auxiliary material Chinese yam
The near infrared spectrum data of broken wall medicine materical crude slice sample, data is divided into calibration set and forecast set；Light harvesting modal data will be corrected import
SIMCA-P 12.0 software carries out Row-Center pretreatment, sets up OPLS-DA qualitative model；Described auxiliary material be dextrin, lactose,
One of magnesium stearate, superfine silica gel powder, microcrystalline cellulose, talcum powder, hydroxypropyl cellulose or starch or any combination；
（3）Starch adulterated Chinese yam broken wall medicine materical crude slice quantitative model is set up：Gather pure Chinese yam broken wall medicine materical crude slice sample, adulterated Chinese yam broken wall
The near infrared spectrum data of medicine materical crude slice sample, data is divided into calibration set and forecast set；Light harvesting modal data will be corrected import
MATLAB 7.0.4 software, sample near infrared spectrum is divided into 10,25,50 subintervals, then carry out respectively two, three,
Four interval combinations computings, screen optimal interval combinations and set up siPLS model；Described starch be cornstarch, wheaten starch or
One of tapioca or any combination.
Preferably, a kind of model differentiating that Chinese yam broken wall medicine materical crude slice is adulterated, method for building up is as follows：
（1）Mix the starch of different proportion in Chinese yam broken wall medicine materical crude slice process, the starch obtaining different adding proportions is adulterated
Chinese yam broken wall medicine materical crude slice sample, described starch is one of cornstarch, wheaten starch or tapioca or any combination；
（2）Mix auxiliary material in Chinese yam broken wall medicine materical crude slice process, obtain adding auxiliary material Chinese yam broken wall medicine materical crude slice sample, described auxiliary material
For one of dextrin, lactose, magnesium stearate, superfine silica gel powder, microcrystalline cellulose, talcum powder, hydroxypropyl cellulose or starch or
Any combination；
（3）The OPLS-DA qualitative model of starch adulterated Chinese yam broken wall medicine materical crude slice sample is set up：Gather pure Chinese yam broken wall medicine materical crude slice sample
Product, step（1）The near infrared spectrum data of adulterated Chinese yam broken wall medicine materical crude slice sample, data is divided into calibration set and forecast set；Will
Calibration set spectroscopic data imports SIMCA-P 12.0 software and is pre-processed and discriminant analysis, the qualitative mould of adulterated Chinese yam broken wall medicine materical crude slice
Type adopts first derivative/MSC preprocess method；OPLS-DA model is verified：Scanning forecast set sample near infrared spectrum, using building
The OPLS-DA model having stood carries out generic prediction to forecast set sample；
（4）The OPLS-DA qualitative model adding auxiliary material Chinese yam broken wall medicine materical crude slice sample is set up：Gather pure Chinese yam broken wall medicine materical crude slice sample
Product, step（2）Add the near infrared spectrum data of auxiliary material Chinese yam broken wall medicine materical crude slice sample, data is divided into calibration set and prediction
Collection；Correction light harvesting modal data is imported SIMCA-P 12.0 software pre-processed and discriminant analysis, adulterated Chinese yam broken wall medicine materical crude slice
Qualitative model adopts Row-Center preprocess method；OPLS-DA model is verified：Scanning forecast set sample near infrared spectrum, adopts
With the OPLS-DA model establishing, generic prediction is carried out to forecast set sample；
（5）The siPLS quantitative model of starch adulterated Chinese yam broken wall medicine materical crude slice sample is set up：The pure Chinese yam broken wall medicine materical crude slice sample of collection,
Step（1）The near infrared spectrum data of adulterated Chinese yam broken wall medicine materical crude slice sample, data is divided into calibration set and forecast set；To correct
Collection spectroscopic data imports MATLAB 7.0.4 software, sample near infrared spectrum is divided into 10,25,50 subintervals, then distinguishes
Carry out two, three, four interval combinations computings, screen optimal interval combinations and set up siPLS model；SiPLS quantitative model is tested
Card：The model built up is imported, calibration set model is tested, checking siPLS model adulterated content of starch to unknown sample
Predictive ability.
Preferably, step（3）The acquisition condition of middle spectroscopic data is using specimen cup diffusing reflection sweep parameter, sampling interval
It is set to 2 nm；Spectral scanning range 1100～2300 nm；Scanning times 32 times.
The present invention, before setting up model, will first prepare starch adulterated Chinese yam broken wall medicine materical crude slice sample it is preferable that described starch
The preparation method of adulterated Chinese yam broken wall medicine materical crude slice sample is：In pure Chinese yam broken wall medicine materical crude slice process mix 10%, 20%, 25%,
30%、40%、50%、55%、60%、70%、75%、80%、95%（w/w）Cornstarch or wheaten starch, obtain adulterated 10%, 20%,
25%、30%、40%、50%、55%、60%、70%、75%、80%、95%（w/w）The Chinese yam broken wall medicine materical crude slice sample of cornstarch, and adulterated
10%、20%、25%、30%、40%、50%、55%、60%、70%、75%、80%、95%（w/w）The Chinese yam broken wall medicine materical crude slice sample of wheaten starch
Product.
The present invention, before setting up model, will first prepare interpolation auxiliary material Chinese yam broken wall medicine materical crude slice sample it is preferable that described interpolation
The preparation method of auxiliary material Chinese yam broken wall medicine materical crude slice sample is：According to 1 in pure Chinese yam broken wall medicine materical crude slice process:1（w/w）Mix auxiliary
Material, auxiliary material is respectively dextrin, lactose, magnesium stearate, superfine silica gel powder, microcrystalline cellulose, talcum powder, hydroxypropyl cellulose, starch.
A kind of method differentiating that Chinese yam broken wall medicine materical crude slice is adulterated, concretely comprises the following steps, gathers Chinese yam broken wall medicine materical crude slice sample to be measured
Near infrared spectrum, is differentiated to the near infrared spectrum of Chinese yam broken wall medicine materical crude slice sample to be measured using the model that the present invention is built, from
And obtain the differentiation result of Chinese yam broken wall medicine materical crude slice sample to be measured.
Compared with prior art, the present invention has the advantages that：
The present invention can directly to Chinese yam broken wall medicine materical crude slice, adulterated situation carries out qualitative and quantitative analysis exactly, saves loaded down with trivial details front place
Reason process, has the conventionals method of analysis such as easy and simple to handle, analysis time is short, environmental protection bad to sample nondestructive unrivaled
Advantage, substantially reduces analytical cycle, reduces experimental cost.
Brief description
Fig. 1 is 40 pure grass crystalline substance Huashan medicine broken wall medicine materical crude slice sample atlas of near infrared spectra.
Fig. 2 is 192 starch adulterated Chinese yam broken wall medicine materical crude slice sample atlas of near infrared spectra.
Fig. 3 is 192 interpolation auxiliary material Chinese yam broken wall medicine materical crude slice sample atlas of near infrared spectra.
Fig. 4 is the OPLS-DA model of adulterated Chinese yam broken wall medicine materical crude slice.
Fig. 5 is sentencing using 82 pure Chinese yam broken wall medicine materical crude slice of OPLS-DA Model checking and starch adulterated Chinese yam broken wall medicine materical crude slice
Other result.
Fig. 6 is the OPLS-DA model of the Chinese yam broken wall medicine materical crude slice adding auxiliary material.
Fig. 7 is the Chinese yam broken wall medicine materical crude slice using 82 pure Chinese yam broken wall medicine materical crude slice of OPLS-DA Model checking and interpolation auxiliary material
Differentiate result.
Fig. 8 is cornstarch adulterated Chinese yam broken wall medicine materical crude slice inspection set quantitative model result.
Fig. 9 is wheaten starch adulterated Chinese yam broken wall medicine materical crude slice inspection set quantitative model result.
Figure 10 is the starch qualitative model set up using PLS-DA method.
Figure 11 is the auxiliary material qualitative model set up using 2 order derivatives pretreatments, OPLS-DA method.
Figure 12 is the auxiliary material qualitative model set up using PLS-DA method.
Figure 13 is the auxiliary material qualitative model set up using SNV pretreatment, OPLS-DA method.
Specific embodiment
With reference to Figure of description and specific embodiment, the present invention is made and further elaborating, described embodiment
It is served only for explaining the present invention, be not intended to limit the scope of the present invention.Test method used in following embodiments is such as no special
Different explanation, is conventional method；The material that used, reagent etc., if no special instructions, for the reagent commercially obtaining
And material.
Embodiment 1
（1）Sample preparation：3 batch totally 40 pure Chinese yam broken wall medicine materical crude slice samples of preparation, all leave and take foot in each batch production process
Amount semi-finished product Chinese yam Ultramicro-powder, is respectively used to the preparation of the adulterated sample of Chinese yam broken wall medicine materical crude slice.
The preparation of cornstarch, wheaten starch adulterated Chinese yam broken wall medicine materical crude slice sample：Cornstarch, wheaten starch respectively press than
Example and above-mentioned 3 batch semi-finished product Chinese yam Ultramicro-powders, according to pure Chinese yam broken wall medicine materical crude slice sample preparation methods, are finally made containing corn
Starch（Wheaten starch）10%、20%、25%、30%、40%、50%、55%、60%、70%、75%、80%、95%（w/w）Adulterated broken wall
Medicine materical crude slice sample.The sample of different adulterated ratios repeats to prepare 8, prepares 2 kinds of starch（Wheaten starch, cornstarch）Adulterated sample
Amount to 192.
Add the preparation of the adulterated sample of various auxiliary material Chinese yam broken wall medicine materical crude slice：Respectively using dextrin, lactose, magnesium stearate, micro-
Powder silica gel, microcrystalline cellulose, talcum powder, hydroxypropyl cellulose, starch and above-mentioned 3 batch semi-finished product Chinese yam Ultramicro-powders are according to pure
Chinese yam broken wall medicine materical crude slice sample preparation methods, being finally made containing auxiliary material proportion is 1:1（w/w）Interpolation different auxiliary material adulterated broken wall
Medicine materical crude slice sample.The sample adding different auxiliary material repeats to prepare 8, and 8 kinds of preparation is added auxiliary material sample and amounted to 192.
（2）Data acquisition：Using Luminar 5030 AOTF near-infrared spectrometers collection sample near infrared spectrum letter
Breath, using specimen cup diffusing reflection sweep parameter, the sampling interval is set to 2nm；Spectral scanning range 1100～2300 nm；Scanning
Number of times 32 times, the near infrared spectrum averaged as sample.40 pure Chinese yam broken wall medicine materical crude slice sample atlas of near infrared spectra are as schemed
1；192 starch adulterated Chinese yam broken wall medicine materical crude slice sample atlas of near infrared spectra such as Fig. 2；192 interpolation auxiliary material Chinese yam broken wall medicine materical crude slice samples
Product atlas of near infrared spectra such as Fig. 3.
（3）Data set divides：By 40 pure Chinese yam broken wall medicine materical crude slice samples and 192 starch adulterated Chinese yam broken wall medicine materical crude slice samples
Totally 232 samples are grouped, and wherein calibration set number is 150, and inspection set is 82.By 40 pure Chinese yam broken wall medicine materical crude slice samples
Product and 192 add auxiliary material Chinese yam broken wall medicine materical crude slice sample totally 232 samples are grouped, and wherein calibration set number is 150, inspection
Test collection and be 82.
（4）Starch adulterated Chinese yam broken wall medicine materical crude slice qualitative analysis：The foundation of OPLS-DA model, correction light harvesting modal data is led
Enter SIMCA-P 12.0 software to be pre-processed and discriminant analysis, using first derivative/MSC (multiplicative scatter correction) pretreatment side
Method, model parameter R2Y=0.866, Q2=0.809.Result such as Fig. 4,3 classification samples can be made a distinction by model well（A
Represent pure Chinese yam broken wall medicine materical crude slice set；B represents cornstarch adulterated Chinese yam broken wall medicine materical crude slice set；It is adulterated broken that C represents wheaten starch
Wall medicine materical crude slice set）, simultaneously it is apparent that mixing pseudo- content of starch with first principal component axle from left to right more and more higher.
Permutation test（n=100）Show that this discrimination model does not have overcoupling defect.
Model testing：Class prediction, result are carried out to 82 pure Chinese yam broken wall medicine materical crude slice and starch adulterated Chinese yam broken wall medicine materical crude slice
It is 100% using OPLS-DA Model checking accuracy, result such as Fig. 5.
（5）Add auxiliary material Chinese yam broken wall medicine materical crude slice qualitative analysis：The foundation of OPLS-DA model, correction light harvesting modal data is led
Enter SIMCA-P 12.0 software to be pre-processed and discriminant analysis, using Row-Center preprocess method, model parameter R2Y=
0.9, Q2=0.832.Result such as Fig. 6,9 classification samples can be made a distinction by model well（A represents pure interpolation dextrin and breaks
Wall medicine materical crude slice set；B represents and adds lactose broken wall medicine materical crude slice set；C represents and adds magnesium stearate broken wall medicine materical crude slice set；D represents and adds
Superfine silica gel powder broken wall medicine materical crude slice set；E represents and adds microcrystalline cellulose broken wall medicine materical crude slice set；F represents and adds talcum powder broken wall medicine materical crude slice
Set；G represents and adds hydroxypropyl cellulose broken wall medicine materical crude slice set；H represents and adds starch broken wall medicine materical crude slice set；J represents pure Chinese yam
Broken wall medicine materical crude slice set）.Permutation test（n=100）Show that this discrimination model does not have overcoupling defect.
Model testing：Class prediction, result are carried out to 82 pure Chinese yam broken wall medicine materical crude slice and auxiliary material adulterated Chinese yam broken wall medicine materical crude slice
It is 100% using OPLS-DA Model checking accuracy, result such as Fig. 7.
（6）The quantitative analysis of the adulterated sample of starch：
The foundation of siPLS model：Light harvesting modal data will be corrected and import MATLAB7.0.4 software, sample near infrared spectrum will be divided
For 10,25,50 subintervals, then carry out two, three, four interval combinations computings respectively, simultaneously with PLS (offset minimum binary
Method), iPLS (interval PLS) analysis result compare, select RMSECV value minimum Method Modeling, result such as table 1,
Table 2.
Table 1 cornstarch adulterated Chinese yam broken wall medicine materical crude slice calibration set PLS model analysis comparative result
aLV is latent variable
Table 2 wheaten starch adulterated Chinese yam broken wall medicine materical crude slice calibration set PLS model analysis comparative result
aLV is latent variable
Com-parison and analysis can draw, sets up cornstarch adulterated Chinese yam broken wall medicine materical crude slice quantitative model using siPLS the most reliable, by sample
Near infrared spectrum is divided into 10 subintervals, during four interval [2,3,6,8], calibration model RMSECV value minimum 1.7872.
Wheaten starch adulterated Chinese yam broken wall medicine materical crude slice quantitative model is set up using siPLS the most reliable, sample near infrared spectrum is divided into 10
Individual subinterval, during four interval [3,4,6,9], calibration model RMSECV value minimum 1.6462.
Model testing：The model built up is imported, calibration set is tested, checking siPLS model is to unknown sample
Predictive ability.Cornstarch adulterated Chinese yam broken wall medicine materical crude slice inspection set model result such as Fig. 8：Calibration set coefficient correlation is 0.9975,
Prediction related coefficient is 0.9980, and predictive ability is good.Wheaten starch adulterated Chinese yam broken wall medicine materical crude slice inspection set model result such as Fig. 9：
Calibration set coefficient correlation is 0.9979, and prediction related coefficient is 0.9971, and predictive ability is good.
The present invention can directly to Chinese yam broken wall medicine materical crude slice, adulterated situation carries out qualitative and quantitative analysis exactly, saves loaded down with trivial details
Pretreatment process, has the conventionals method of analysis such as easy and simple to handle, analysis time is short, environmental protection bad to sample nondestructive no comparable
The advantage intended, substantially reduces analytical cycle, reduces cost.
Comparative example 1
This comparative example, when setting up starch adulterated Chinese yam broken wall draft qualitative analysis model, sets up method and the embodiment 1 of model
Difference, uses PLS-DA model, and, with embodiment 1, the model result finally obtaining is as shown in Figure 10 for other.Foundation is described
Model is unstable.
Comparative example 2
This comparative example set up add auxiliary material Chinese yam broken wall draft qualitative analysis model when, the preprocess method of data and embodiment
1 is different, use 2 order derivatives and process,, with embodiment 1, the model result finally obtaining is as shown in figure 11 for other.Illustrate to set up
Model unstable.
Comparative example 3
This comparative example, when setting up interpolation auxiliary material Chinese yam broken wall draft qualitative analysis model, sets up method and the embodiment 1 of model
Difference, uses PLS-DA model, and, with embodiment 1, the model result finally obtaining is as shown in figure 12 for other.Foundation is described
Model is unstable.
Comparative example 4
This comparative example set up add auxiliary material Chinese yam broken wall draft qualitative analysis model when, the preprocess method of data and embodiment
1 is different, use SNV process,, with embodiment 1, the model result finally obtaining is as shown in figure 13 for other.The mould set up is described
Type is unstable.
Claims (4)
1. a kind of model differentiating that Chinese yam broken wall medicine materical crude slice is adulterated is it is characterised in that method for building up is as follows：
（1）Starch adulterated Chinese yam broken wall medicine materical crude slice qualitative model is set up：Gather pure Chinese yam broken wall medicine materical crude slice sample, adulterated Chinese yam broken wall
The near infrared spectrum data of medicine materical crude slice sample, data is divided into calibration set and forecast set；Light harvesting modal data will be corrected import
SIMCA-P 12.0 software carries out first derivative/MSC pretreatment, sets up OPLS-DA qualitative model；Described starch forms sediment for corn
One of powder, wheaten starch or tapioca or any combination；
（2）Add auxiliary material Chinese yam broken wall medicine materical crude slice qualitative model to set up：Gather pure Chinese yam broken wall medicine materical crude slice sample, add auxiliary material Chinese yam
The near infrared spectrum data of broken wall medicine materical crude slice sample, data is divided into calibration set and forecast set；Light harvesting modal data will be corrected import
SIMCA-P 12.0 software carries out Row-Center pretreatment, sets up OPLS-DA qualitative model；Described auxiliary material be dextrin, lactose,
One of magnesium stearate, superfine silica gel powder, microcrystalline cellulose, talcum powder, hydroxypropyl cellulose or starch or any combination；
（3）Starch adulterated Chinese yam broken wall medicine materical crude slice quantitative model is set up：Gather pure Chinese yam broken wall medicine materical crude slice sample, adulterated Chinese yam broken wall
The near infrared spectrum data of medicine materical crude slice sample, data is divided into calibration set and forecast set；Light harvesting modal data will be corrected import
MATLAB 7.0.4 software, sample near infrared spectrum is divided into 10,25,50 subintervals, then carry out respectively two, three,
Four interval combinations computings, screen optimal interval combinations and set up siPLS model；Described starch be cornstarch, wheaten starch or
One of tapioca or any combination.
2. according to claim 1 model it is characterised in that method for building up is as follows：
（1）Mix the starch of different proportion in Chinese yam broken wall medicine materical crude slice process, the starch obtaining different adding proportions is adulterated
Chinese yam broken wall medicine materical crude slice sample, described starch is one of cornstarch, wheaten starch or tapioca or any combination；
（2）Mix auxiliary material in Chinese yam broken wall medicine materical crude slice process, obtain adding auxiliary material Chinese yam broken wall medicine materical crude slice sample, described auxiliary material
For one of dextrin, lactose, magnesium stearate, superfine silica gel powder, microcrystalline cellulose, talcum powder, hydroxypropyl cellulose or starch or
Any combination；
（3）The OPLS-DA qualitative model of starch adulterated Chinese yam broken wall medicine materical crude slice sample is set up：Gather pure Chinese yam broken wall medicine materical crude slice sample
Product, step（1）The near infrared spectrum data of adulterated Chinese yam broken wall medicine materical crude slice sample, data is divided into calibration set and forecast set；Will
Calibration set spectroscopic data imports SIMCA-P 12.0 software and is pre-processed and discriminant analysis, the qualitative mould of adulterated Chinese yam broken wall medicine materical crude slice
Type adopts first derivative/MSC preprocess method；OPLS-DA model is verified：Scanning forecast set sample near infrared spectrum, using building
The OPLS-DA model having stood carries out generic prediction to forecast set sample；
（4）The OPLS-DA qualitative model adding auxiliary material Chinese yam broken wall medicine materical crude slice sample is set up：Gather pure Chinese yam broken wall medicine materical crude slice sample
Product, step（2）Add the near infrared spectrum data of auxiliary material Chinese yam broken wall medicine materical crude slice sample, data is divided into calibration set and prediction
Collection；Correction light harvesting modal data is imported SIMCA-P 12.0 software pre-processed and discriminant analysis, adulterated Chinese yam broken wall medicine materical crude slice
Qualitative model adopts Row-Center preprocess method；OPLS-DA model is verified：Scanning forecast set sample near infrared spectrum, adopts
With the OPLS-DA model establishing, generic prediction is carried out to forecast set sample；
（5）The siPLS quantitative model of starch adulterated Chinese yam broken wall medicine materical crude slice sample is set up：The pure Chinese yam broken wall medicine materical crude slice sample of collection,
Step（1）The near infrared spectrum data of adulterated Chinese yam broken wall medicine materical crude slice sample, data is divided into calibration set and forecast set；To correct
Collection spectroscopic data imports MATLAB 7.0.4 software, sample near infrared spectrum is divided into 10,25,50 subintervals, then distinguishes
Carry out two, three, four interval combinations computings, screen optimal interval combinations and set up siPLS model；SiPLS quantitative model is tested
Card：The model built up is imported, calibration set model is tested, checking siPLS model adulterated content of starch to unknown sample
Predictive ability.
3. model according to claim 1 and 2 is it is characterised in that step（3）The acquisition condition of middle spectroscopic data is use
Specimen cup diffusing reflection sweep parameter, the sampling interval is set to 2 nm；Spectral scanning range 1100～2300 nm；Scanning times 32
Secondary.
4. a kind of method differentiating that Chinese yam broken wall medicine materical crude slice is adulterated is it is characterised in that gather the near of Chinese yam broken wall medicine materical crude slice sample to be measured
Infrared spectrum, is entered to the near infrared spectrum of Chinese yam broken wall medicine materical crude slice sample to be measured using the model described in any one of claim 1 to 3
Row differentiates, thus obtaining the differentiation result of Chinese yam broken wall medicine materical crude slice sample to be measured.
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Application publication date: 20170215 Assignee: Guangdong Cao Jinghua wall breaking herbaceous Co.,Ltd. Assignor: ZHONGSHAN ZEUS MEDICINE GROUP Co.,Ltd. Contract record no.: X2020440000098 Denomination of invention: A method of discriminating common yam rhizome wall-broken decoction piece adulteration Granted publication date: 20190830 License type: Common License Record date: 20200622 |