CN103411895B - Pseudo-near infrared spectrum identification method mixed by pearl powder - Google Patents
Pseudo-near infrared spectrum identification method mixed by pearl powder Download PDFInfo
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Abstract
The invention discloses a kind of pearl powder and mix pseudo-near infrared spectrum identification method.The present invention's application Fourier transform near infrared diffuse reflectance spectroscopy analytical technology is in conjunction with the method for qualitative analysis of similarity mode analysis (Similarity Match Analysis), and the similarity mode mixing pseudo-pearl powder setting up the general impurity of doping differentiates model; Application Fourier transform near infrared diffuse reflectance spectroscopy analytical technology is in conjunction with partial least square method (Partial Least Squares, PLS) quantitative analysis method, set up the quantitative discriminating model of pearl powder massfraction in the pearl powder for doping oyster shell whiting, and realize pearl powder with two models couplings application and mix pseudo-effectively differentiating fast: that adulterates general impurity by similarity mode analysis and identification mixes pseudo-pearl powder; By quantitative test differentiate doping oyster shell whiting mix pseudo-pearl powder.
Description
Technical field
The present invention relates to pearl powder and mix pseudo-near infrared spectrum identification method.
Background technology
Pearl powder in recent years as rare traditional Chinese medicine enjoys favor in industries such as medicine, health food, cosmetics, and commercialized product kind is further abundant, application is constantly widened, economic worth is growing, but fake and forged pearl powder also arises at the historic moment.Mother-of-pearl shell and pearl are with root homology, the microscopic appearance of mother-of-pearl oyster shell whiting is similar to pearl powder with chemical composition, often pretend to be pearl powder or mix in pearl powder and come into the market, even there is powder like other outer appearnces, as shell of seaear powder, talcum powder, Paris white etc., impurity is doped in pearl powder or pretends to be pearl powder to come into the market, these fake and inferior pearl powder very disruptive pearl powder market orders, affect consumer physical and mental health and hinder the sound development of pearl powder industry.
Existing research adopts the method such as thermal analysis system, X-ray diffraction method, infra-red sepectrometry, scanning electron microscopy to differentiate the crystal phase structure of mother-of-pearl oyster shell whiting and oyster shell whiting and pearl powder, microscopic pattern and content of organic matter difference, but morphology analysis can not effectively differentiate oyster shell whiting and pearl powder, and crystal phase structure and organic analysis need to carry out pyroprocessing to study the transformation difference of process front and back to realize differentiating to pearl powder and adulterant thereof usually.Such as application number is 200910099718.X, publication number is the discrimination method that the Chinese patent application of CN101620176 discloses a kind of pearl powder and oyster shell whiting, it needs to be mixed and made into transparent sheet with potassium bromide respectively by after pearl powder and oyster shell whiting calcining, and the characteristic peak then by measuring infrared spectrum distinguishes pearl powder and oyster shell whiting.These methods need accurate pre-processing device or annex and large-sized analytic instrument to carry out analyzing and data processing usually, and thermal treatment and follow-up data process need certain hour, and therefore these methods do not have the feature such as agility, simplicity.
Near infrared spectrum (Near Infrared Spectroscopy, NIRS) analyzing is the material information utilizing near infrared spectrum district to comprise, for a kind of analytical approach of measured object qualitative and quantitative analysis, do not need the advantages such as pre-service and multicomponent detect simultaneously because it has quick, pollution-free, sample and be applied to the qualitative and quantitative analysis of medicinal material medicine more and more.The characteristic of near-infrared spectrum analysis needed to set up classification and quantitative model before analysis sample, although find suitable modeling pattern and be not easy, modeling process needs certain hour usually, but after corresponding model has been set up, near-infrared spectral analytical method will become a kind of easy, reliable rapid analysis.
Summary of the invention
The object of this invention is to provide and differentiate that the method for building up of pseudo-near-infrared diffuse reflection spectrum analytical model mixed by pearl powder, and pseudo-near infrared spectrum identification method mixed by the pearl powder based on this.
Pseudo-near infrared spectrum identification method mixed by pearl powder provided by the invention, can apply Fourier transform near infrared diffuse reflectance spectroscopy analytical technology and differentiate generally to mix pseudo-pearl powder in conjunction with the qualitative analysis model that similarity mode analysis is set up.
The massfraction of pearl powder in the pearl powder of the Quantitative Analysis Model quantitative forecast doping oyster shell whiting that Fourier transform near infrared diffuse reflectance spectroscopy analytical technology is set up in conjunction with partial least square method can also be applied to differentiate to mix pseudo-pearl powder.
Preferred scheme is:
Choose pure pearl powder sample and pure oyster shell whiting sample as calibration set;
Use Fourier Transform Near Infrared instrument (FT-NIR) and supporting spectral analysis software thereof gather spectroscopic data and set up analytical model, spectra collection condition comprises: integrating sphere diffuse reflectance accessory; Spectral range 4000-10000cm
-1;
At least 10 pure pearl powder samples are chosen as calibration set in the foundation of similarity mode analytical model, near infrared spectrum software is used to set up similarity mode analytical model: light path type selecting multicomponent signal corrects (Multiplicative Signal Correction, MSC); Pretreated spectra adopts second derivative; The filtering of level and smooth employing Norris derivative; SPECTRAL REGION is at 4000-10000cm
-1in scope.
Mix pseudo-pearl powder massfraction quantitatively differentiate the mode adopting pure pearl powder and pure oyster shell whiting to mix mutually in the foundation of model simulate doping oyster shell whiting mix pseudo-pearl powder, accurately take pearl powder and oyster shell whiting mixes, and control biased sample gross mass at more than 5g, using the massfraction of pearl powder in biased sample as the qualitative characteristics quantitative parameter of biased sample, the pearl powder massfraction of doped samples is calculated by doping ratio, pure pearl powder massfraction is defined as 100% simultaneously, pure oyster shell whiting massfraction is defined as 0%, choose simulation and mix pseudo-sample and corresponding pearl powder and oyster shell whiting sterling jointly as calibration set, partial least square method is used to set up Quantitative Analysis Model: light path type selecting multicomponent signal corrects, Pretreated spectra adopts second derivative, the filtering of level and smooth employing Norris derivative, SPECTRAL REGION is at 4000-10000cm
-1in scope.
Sample preferably carries out drying and fully grinding before carrying out near infrared spectrum test.
Such as: in baking oven at 50 DEG C dry 12h with reduce moisture on test impact; Reunite on the impact of test to reduce sample with the abundant ground sample of agate mortar.
Preferred spectra collection condition also comprises: resolution 8cm
-1; Scanning times 64 times; Use the gain parameter of instrument Automatic Optimal.
With regard to provided by the invention for differentiating that the method for building up of pseudo-analytical model mixed by pearl powder, it comprises qualitative analysis model and Quantitative Analysis Model:
Described qualitative analysis model application Fourier transform near infrared diffuse reflectance spectroscopy analytical technology is set up in conjunction with similarity mode analysis;
Described Quantitative Analysis Model application Fourier transform near infrared diffuse reflectance spectroscopy analytical technology is set up in conjunction with partial least square method;
Choose pure pearl powder sample and pure oyster shell whiting sample as calibration set;
Use Fourier Transform Near Infrared instrument and supporting spectral analysis software thereof gather spectroscopic data and set up analytical model, spectra collection condition comprises: integrating sphere diffuse reflectance accessory; Spectral range 4000-10000cm
-1;
Choose at least 10 pure pearl powder samples in the foundation of similarity mode analytical model as calibration set, use near infrared spectrum software to set up similarity mode analytical model: light path type selecting multicomponent signal corrects; Pretreated spectra adopts second derivative; The filtering of level and smooth employing Norris derivative; SPECTRAL REGION is at 4000-10000cm
-1in scope.
Mix pseudo-pearl powder massfraction quantitatively differentiate the mode adopting pure pearl powder and pure oyster shell whiting to mix mutually in the foundation of model simulate doping oyster shell whiting mix pseudo-pearl powder, accurately take pearl powder and oyster shell whiting mixes, and control biased sample gross mass at more than 5g, using the massfraction of pearl powder in biased sample as the qualitative characteristics quantitative parameter of biased sample, the pearl powder massfraction of doped samples is calculated by doping ratio, pure pearl powder massfraction is defined as 100% simultaneously, pure oyster shell whiting massfraction is defined as 0%, choose simulation and mix pseudo-sample and corresponding pearl powder and oyster shell whiting sterling jointly as calibration set, partial least square method is used to set up Quantitative Analysis Model: light path type selecting multicomponent signal corrects, Pretreated spectra adopts second derivative, the filtering of level and smooth employing Norris derivative, SPECTRAL REGION is at 4000-10000cm
-1in scope.
Except described modeling method and the method utilizing the described analytical model discriminating pearl powder true and false; the analytical model of described method establishment itself is also the part that the present invention will protect, and the present invention also relates to the analytical model of described method establishment for differentiating that pseudo-purposes mixed by pearl powder.
Utilize institute of the present invention established model quantitatively to differentiate for the purity of mixing pseudo-pearl powder of the oyster shell whiting that adulterates, can rapid and accurate determination doping oyster shell whiting the massfraction mixing pearl powder in pseudo-pearl powder.
Accompanying drawing explanation
Fig. 1 is the near infrared light spectrogram of similarity analysis model pearl powder calibration set.
Fig. 2 is the near infrared light spectrogram of Quantitative Analysis Model simulation doping pearl powder calibration set.
Fig. 3 is that Quantitative Analysis Model pearl powder corrects and checking correlogram.
Fig. 4 is Quantitative Analysis Model cross validation correlogram.
Embodiment
The present invention's application Fourier transform near infrared diffuse reflectance spectroscopy analytical technology is in conjunction with the method for qualitative analysis of similarity mode analysis (Similarity MatchAnalysis), and the similarity mode setting up pearl powder differentiates model; Application Fourier transform near infrared diffuse reflectance spectroscopy analytical technology is in conjunction with partial least square method (Partial Least Squares, PLS) quantitative analysis method, set up the quantitative discriminating model of pearl powder for doping oyster shell whiting, and realize pearl powder with two models couplings application and mix pseudo-effectively differentiating fast: that adulterates general impurity by similarity mode analysis and identification mixes pseudo-pearl powder; By quantitative test differentiate doping oyster shell whiting mix pseudo-pearl powder.Below modeling method and application thereof are illustrated.
Choose 10 batches, the pure pearl powder sample of fine qualities coming from Zhejiang Province's Zhuji City, number consecutively is Z-1 to Z-10; Pure mother-of-pearl oyster shell whiting 4 batches, number consecutively is B-1 to B-4.Before sample carries out near infrared spectrum test, in baking oven at 50 DEG C dry 12h with reduce moisture on test impact; Reunite on the impact of test to reduce sample with the abundant ground sample of agate mortar.
Use the FT-NIR Analyzer that instrument is Thermo Scientific company model Antaris II, spectral analysis software is Thermo Scientific company's T Q Analyst 9.0.Spectra collection condition is: integrating sphere diffuse reflectance accessory; Spectral range 4000-10000cm
-1; Resolution 8cm
-1; Scanning times 64 times; Instrument Automatic Optimal empty door is decayed, and gain is 2.
The foundation of similarity mode analytical model: choose pearl powder sample Z-1 to Z-10 as calibration set, according to the near infrared light spectrogram (as shown in Figure 1) of above-mentioned condition successively collected specimens Z-1 to Z-10.Use TQ Analyst 9.0 to set up similarity mode analytical model, design parameter arranges as follows:
Analysis type (Analysis Type): selection sort (Classification), similarity mode (Similarity Match);
Light path type (Pathlength Type): select multicomponent signal to correct (Multiplicative Signal Correction, MSC);
Standard (Standards): import the calibration set sample near infrared light spectrogram gathered;
Spectrum (Spectra): subtraction of spectra computing (Spectral Subtraction) is selected without computing (No Subtraction),
Data mode (Data Format) selects second derivative (Second Derivative) pre-service (ProcessStandards),
Smoothly (Smoothing) selects Norris derivative filtering (Norris Derivative Filter), parameter (Segment Length5, Gap Between Segments5),
Multiple spot baseline correction (Multipoint Baseline Correction) is selected without correcting (No Correction);
SPECTRAL REGION (Regions): editor's (Edit) SPECTRAL REGION is 4100-9800cm
-1.
Other parameters all adopt default setting.
Choose commercially available natural ostreae testa pulverata, commercially available shell of seaear powder (prepared slices of Chinese crude drugs grind into powder), talcum powder (chemically pure reagent) and commercially available nanometer grade calcium carbonate powder as simulation personation pearl powder, and pearl powder Z-10 is adulterated as mixing pseudo-pearl powder with nano-calcium carbonate, natural ostreae testa pulverata respectively in proportion, as shown in table 1.The similarity analysis model that application is set up is mixed pseudo-sample to above-mentioned simulation and is analyzed, and result (see table 1) shows that this model can differentiate the pearl powder that general impurity adulterates fast.
Table 1
Mix the foundation that model quantitatively differentiated by pseudo-pearl powder: choose pearl powder sample and each four of oyster shell whiting sample, accurately take pearl powder and oyster shell whiting mixes, and controlling biased sample gross mass at 5g, biased sample agate grinding fully grinding is to be measured to mix.Be specially that pearl powder Z-1 and oyster shell whiting B-1 adulterates mutually, pearl powder Z-2 and oyster shell whiting B-2 adulterates mutually, pearl powder Z-3 and oyster shell whiting B-3 adulterates mutually, obtain a series of simulation and mix pseudo-sample, number consecutively is C-1 to C-25, calculate the massfraction of pearl powder in biased sample, as shown in table 2; Mutually adulterated by pearl powder Z-4 and oyster shell whiting B-4, obtain a series of simulation and mix pseudo-testing sample, number consecutively is V-1 to V-4, calculates the massfraction of pearl powder in testing sample, as shown in table 3.
Table 2
Choose analog sample C-1 to C-25, pure pearl powder sample Z-1 to Z-3, pure oyster shell whiting sample B-1 to B-3 jointly as calibration set, according to the near infrared light spectrogram (as shown in Figure 2) of aforementioned condition successively acquisition correction collection sample; Choose testing sample V-1 to V-4 as checking collection, gather near infrared spectrum according to the same terms.Use TQ Analyst 9.0 software to set up Quantitative Analysis Model, design parameter arranges as follows:
Analysis type (Analysis Type): select quantitative test (Quantitative analysis), partial least square method (Partial LeastSquares, PLS);
Light path type (Pathlength Type): select multicomponent signal to correct (Multiplicative Signal Correction, MSC);
Component (Components): definition " pearl powder content " for Component, Unit be " % ";
Standard (Standards): import the calibration set sample near infrared light spectrogram gathered;
Spectrum (Spectra): subtraction of spectra computing (Spectral Subtraction) is selected without computing (No Subtraction),
Data mode (Data Format) selects second derivative (Second Derivative) pre-service (ProcessStandards),
Smoothly (Smoothing) selects Norris derivative filtering (Norris Derivative Filter), parameter (Segment Length5, Gap Between Segments5), multiple spot baseline correction (Multipoint Baseline Correction) is selected without correcting (No Correction);
SPECTRAL REGION (Regions): editor's (Edit) SPECTRAL REGION is 4100-9800cm
-1.
Other parameters all adopt default setting.
The correction of institute's established model and checking correlogram (Calibration, calibration set; Validation, checking collection) as shown in Figure 3, calibration set related coefficient is 0.9999, correcting mean square deviation (RMSEC) is 0.411; Prediction related coefficient is 0.9998, and prediction mean square deviation (RMSEP) is 1.72.As shown in Figure 4, calibration set cross validation mean square deviation (RMSECV) is 4.53 to cross validation results, and related coefficient is 0.9903.Checking is concentrated and is mixed pearl powder massfraction in pseudo-pearl powder and pure pearl powder and to predict the outcome deviation between (see table 3) and actual computation value less (<5%), institute's established model can quick and precisely predict doping oyster shell whiting the massfraction mixing pearl powder in pseudo-pearl powder, and with this differentiate survey pearl powder purity and quality.
Table 3
Above embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that the common engineering technical personnel in this area make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determine.
Claims (6)
1. pseudo-near infrared spectrum identification method mixed by pearl powder, it is characterized in that applying Fourier transform near infrared diffuse reflectance spectroscopy analytical technology differentiates generally to mix pseudo-pearl powder in conjunction with the qualitative analysis model that similarity mode analysis is set up;
In the pearl powder of the Quantitative Analysis Model quantitative measurement doping oyster shell whiting that application Fourier transform near infrared diffuse reflectance spectroscopy analytical technology is set up in conjunction with partial least square method, the massfraction of pearl powder is to differentiate to mix pseudo-pearl powder;
Choose pure pearl powder sample and pure oyster shell whiting sample as calibration set;
Use Fourier Transform Near Infrared instrument and supporting spectral analysis software thereof gather spectroscopic data and set up analytical model, spectra collection condition comprises: integrating sphere diffuse reflectance accessory; Spectral range 4000-10000cm
-1;
Choose at least 10 pure pearl powder samples in the foundation of similarity mode analytical model as calibration set, use near infrared spectrum software to set up similarity mode analytical model: light path type selecting multicomponent signal corrects; Pretreated spectra adopts second derivative; The filtering of level and smooth employing Norris derivative; SPECTRAL REGION is at 4000-10000cm
-1in scope;
Mix pseudo-pearl powder massfraction quantitatively differentiate the mode adopting pure pearl powder and pure oyster shell whiting to mix mutually in the foundation of model simulate doping oyster shell whiting mix pseudo-pearl powder, accurately take pearl powder and oyster shell whiting mixes, and control biased sample gross mass at more than 5g, using the massfraction of pearl powder in biased sample as the qualitative characteristics quantitative parameter of biased sample, the pearl powder massfraction of doped samples is calculated by doping ratio, pure pearl powder massfraction is defined as 100% simultaneously, pure oyster shell whiting massfraction is defined as 0%, choose simulation and mix pseudo-sample and corresponding pearl powder and oyster shell whiting sterling jointly as calibration set, partial least square method is used to set up Quantitative Analysis Model: light path type selecting multicomponent signal corrects, Pretreated spectra adopts second derivative, the filtering of level and smooth employing Norris derivative, SPECTRAL REGION is at 4000-10000cm
-1in scope.
2. pseudo-near infrared spectrum identification method mixed by pearl powder according to claim 1, it is characterized in that, sample carries out drying and fully grinding before carrying out near infrared spectrum test.
3. pseudo-near infrared spectrum identification method mixed by pearl powder according to claim 2, it is characterized in that, in baking oven at 50 DEG C dry 12h to reduce moisture to the impact tested; Reunite on the impact of test to reduce sample with the abundant ground sample of agate mortar.
4. pseudo-near infrared spectrum identification method mixed by pearl powder according to claim 1, and it is characterized in that, spectra collection condition also comprises: resolution 8cm
-1; Scanning times 64 times; Use the gain parameter of instrument Automatic Optimal.
5., for differentiating that the method for building up of pseudo-analytical model mixed by pearl powder, it is characterized in that, described analytical model comprises qualitative analysis model and Quantitative Analysis Model,
Described qualitative analysis model application Fourier transform near infrared diffuse reflectance spectroscopy analytical technology is set up in conjunction with similarity mode analysis;
Described Quantitative Analysis Model application Fourier transform near infrared diffuse reflectance spectroscopy analytical technology is set up in conjunction with partial least square method;
Choose pure pearl powder sample and pure oyster shell whiting sample as calibration set;
Use Fourier Transform Near Infrared instrument and supporting spectral analysis software thereof gather spectroscopic data and set up analytical model, spectra collection condition comprises: integrating sphere diffuse reflectance accessory; Spectral range 4000-10000cm
-1;
Choose at least 10 pure pearl powder samples in the foundation of similarity mode analytical model as calibration set, use near infrared spectrum software to set up similarity mode analytical model: light path type selecting multicomponent signal corrects; Pretreated spectra adopts second derivative; The filtering of level and smooth employing Norris derivative; SPECTRAL REGION is at 4000-10000cm
-1in scope;
Mix pseudo-pearl powder massfraction quantitatively differentiate the mode adopting pure pearl powder and pure oyster shell whiting to mix mutually in the foundation of model simulate doping oyster shell whiting mix pseudo-pearl powder, accurately take pearl powder and oyster shell whiting mixes by a certain percentage, and control biased sample gross mass at more than 5g, using the massfraction of pearl powder in biased sample as the qualitative characteristics quantitative parameter of biased sample, the pearl powder massfraction of doped samples is calculated by doping ratio, pure pearl powder massfraction is defined as 100% simultaneously, pure oyster shell whiting massfraction is defined as 0%, choose simulation and mix pseudo-sample and corresponding pearl powder and oyster shell whiting sterling jointly as calibration set, partial least square method is used to set up Quantitative Analysis Model: light path type selecting multicomponent signal corrects, Pretreated spectra adopts second derivative, the filtering of level and smooth employing Norris derivative, SPECTRAL REGION is at 4000-10000cm
-1in scope.
6. the analytical model of method establishment according to claim 5 is for differentiating that pseudo-purposes mixed by pearl powder.
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| CN103837492B (en) * | 2014-02-24 | 2015-11-25 | 西北农林科技大学 | A kind of Kiwi berry based on near-infrared spectrum technique expand fruit lossless detection method |
| CN107727591A (en) * | 2017-09-27 | 2018-02-23 | 天津工业大学 | A kind of ternary based on integrating sphere diffusing reflection uv-vis spectra mixes pseudo- pseudo-ginseng quantitative analysis method |
| CN109444186A (en) * | 2018-12-25 | 2019-03-08 | 浙江大学 | A kind of pearl powder X-ray diffraction differential method |
| CN111337448B (en) * | 2020-03-26 | 2023-05-12 | 杭州老爸评测科技股份有限公司 | Method for identifying cosmetics based on infrared spectrum technology |
| CN114486789A (en) * | 2022-01-13 | 2022-05-13 | 广西爱呗利生物科技有限公司 | Method for constructing fingerprint spectrum of pearl layer powder hydrogel patch and fingerprint spectrum thereof |
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