CN103411895A - Near infrared spectrum identification method of adulteration of pearl powder - Google Patents
Near infrared spectrum identification method of adulteration of pearl powder Download PDFInfo
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Abstract
The invention discloses a near infrared spectrum identification method of the adulteration of pearl powder. According to the near infrared spectrum identification method, a Fourier transform near-infrared diffuse reflection spectrum analysis technology is combined with a qualitative analysis method of similarity match analysis so as to establish a similarity match identification model of adulterated pearl powder doped with common impurities; the Fourier transform near-infrared diffuse reflection spectrum analysis technology is combined with a PLS (partial least squares) quantitative analysis method to establish a quantitative identification model aiming at the mass percentage of the pearl powder in the pearl powder doped with shell powder; the two models are combined to realize rapid and effective identification of the adulteration of the pearl powder, wherein the adulterated pearl powder doped with the common impurities is identified by the similarity match analysis, and the adulterated pearl powder doped with the shell powder is identified by quantitative analysis.
Description
Technical field
The present invention relates to pearl powder and mix pseudo-near infrared spectrum identification method.
Background technology
Pearl powder as rare traditional Chinese medicine enjoys favor in industries such as medicine, health food, cosmetics in recent years, and the listing product category is further abundant, application is constantly widened, economic worth is growing, yet fake and forged pearl powder also arises at the historic moment.Mother-of-pearl shell and pearl are with the root homology, the microscopic appearance of mother-of-pearl shell powder is similar to pearl powder with chemical composition, often pretend to be pearl powder or mix in pearl powder and come into the market, powder like other outer appearnces is even arranged, impurity is doped in pearl powder or pretends to be pearl powder to come into the market as shell of seaear powder, talcum powder, Paris white etc., and these fake and inferior pearl powders seriously upset the pearl powder market order, affect the physically and mentally healthy of consumer and hindered the sound development of pearl powder industry.
Existing research adopts the methods such as thermal analysis system, X-ray diffraction method, infra-red sepectrometry, scanning electron microscopy to differentiate that mother-of-pearl shell powder is crystal phase structure, microscopic pattern and the content of organic matter difference of oyster shell whiting and pearl powder, but morphology analysis can not effectively be differentiated oyster shell whiting and pearl powder, and crystal phase structure and organic analyze usually need to be carried out the transformation difference of pyroprocessing before and after processing with research to pearl powder and adulterant thereof and differentiated realizing.For example 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 need to, by after pearl powder and oyster shell whiting calcining, with potassium bromide, being mixed and made into transparent sheet respectively, then distinguish pearl powder and oyster shell whiting by the characteristic peak of measuring infrared spectrum.These methods usually need accurate pre-processing device or annex and large-sized analytic instrument to analyze and data are processed, and thermal treatment and follow-up data processing need certain hour, so these methods do not have the characteristics such as agility, simplicity.
Near infrared spectrum (Near Infrared Spectroscopy, NIRS) analyzing is the material information that utilizes the near infrared spectrum district to comprise, for a kind of analytical approach of measured object qualitative and quantitative analysis, because having quick, pollution-free, sample, it does not need the advantages such as pre-service and multicomponent detect simultaneously to be applied to more and more the qualitative and quantitative analysis of medicinal material medicine.The characteristic of near-infrared spectrum analysis is before analytic sample, to need to set up classification and quantitative model, although find suitable modeling pattern and be not easy, modeling process needs certain hour usually, after but 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 purpose of this invention is to provide the discriminating pearl powder and mix the method for building up of pseudo-near-infrared diffuse reflection spectrum analytical model, and mix pseudo-near infrared spectrum identification method based on this pearl powder.
Pearl powder provided by the invention is mixed pseudo-near infrared spectrum identification method, can apply the Fourier transform near infrared diffuse reflectance spectroscopy analytical technology and differentiate and generally mix pseudo-pearl powder in conjunction with the qualitative analysis model of similarity the matching analysis foundation.
Can also apply the Fourier transform near infrared diffuse reflectance spectroscopy analytical technology and with discriminating, mix pseudo-pearl powder in conjunction with the massfraction of pearl powder in the pearl powder of the Quantitative Analysis Model quantitative forecast doping oyster shell whiting of partial least square method foundation.
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, the spectra collection condition comprises: the integrating sphere diffuse reflectance accessory; Spectral range 4000-10000cm
-1
In the foundation of similarity the matching analysis model, choose at least 10 pure pearl powder samples as calibration set, use near infrared spectrum software to set up similarity the matching analysis model: light path type selecting multicomponent signal is proofreaied and correct (Multiplicative Signal Correction, MSC); Second derivative is adopted in the spectrum pre-service; The filtering of level and smooth employing Norris derivative; SPECTRAL REGION is at 4000-10000cm
-1In scope.
Mixing pseudo-pearl powder massfraction quantitatively differentiates in the foundation of model and to adopt pure pearl powder and the mode that pure oyster shell whiting mixes mutually to simulate the pseudo-pearl powder of mixing of doping oyster shell whiting, accurately take pearl powder and oyster shell whiting mixes, and control the biased sample gross mass more than 5g, using the qualitative characteristics quantitative parameter of the massfraction of pearl powder in biased sample as biased sample, the pearl powder massfraction of doped samples is calculated by doping ratio, simultaneously pure pearl powder massfraction is defined as to 100%, 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, use partial least square method to set up Quantitative Analysis Model: light path type selecting multicomponent signal is proofreaied and correct, second derivative is adopted in the spectrum pre-service, the filtering of level and smooth employing Norris derivative, SPECTRAL REGION is at 4000-10000cm
-1in scope.
Sample carries out preferably carrying out drying and fully grinding before the near infrared spectrum test.
For example: in baking oven under 50 ℃ dry 12h to reduce the impact of moisture on test; With the abundant ground sample of agate mortar, reunite on the impact of test to reduce sample.
Preferred spectra collection condition also comprises: resolution 8cm
-1Scanning times 64 times; Use the gain parameter of instrument Automatic Optimal.
Be used to differentiating that pearl powder mixes the method for building up of pseudo-analytical model, it comprises qualitative analysis model and Quantitative Analysis Model with regard to provided by the invention:
Described qualitative analysis model application Fourier transform near infrared diffuse reflectance spectroscopy analytical technology is set up in conjunction with the similarity the matching 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, the spectra collection condition comprises: the integrating sphere diffuse reflectance accessory; Spectral range 4000-10000cm
-1
In the foundation of similarity the matching analysis model, choose at least 10 pure pearl powder samples as calibration set, use near infrared spectrum software to set up similarity the matching analysis model: light path type selecting multicomponent signal is proofreaied and correct; Second derivative is adopted in the spectrum pre-service; The filtering of level and smooth employing Norris derivative; SPECTRAL REGION is at 4000-10000cm
-1In scope.
Mixing pseudo-pearl powder massfraction quantitatively differentiates in the foundation of model and to adopt pure pearl powder and the mode that pure oyster shell whiting mixes mutually to simulate the pseudo-pearl powder of mixing of doping oyster shell whiting, accurately take pearl powder and oyster shell whiting mixes, and control the biased sample gross mass more than 5g, using the qualitative characteristics quantitative parameter of the massfraction of pearl powder in biased sample as biased sample, the pearl powder massfraction of doped samples is calculated by doping ratio, simultaneously pure pearl powder massfraction is defined as to 100%, 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, use partial least square method to set up Quantitative Analysis Model: light path type selecting multicomponent signal is proofreaied and correct, second derivative is adopted in the spectrum pre-service, the filtering of level and smooth employing Norris derivative, SPECTRAL REGION is at 4000-10000cm
-1in scope.
Except described modeling method and the method for utilizing the described analytical model discriminating pearl powder true and false; the analytical model itself that described method is set up is also the part that the present invention will protect, and the analytical model that the present invention also relates to described method foundation is mixed pseudo-purposes be used to differentiating pearl powder.
Utilize institute of the present invention established model quantitatively to differentiate be used to the purity of mixing pseudo-pearl powder of the oyster shell whiting that adulterates, can rapid and accurate determination the massfraction of mixing pearl powder in pseudo-pearl powder of doping oyster shell whiting.
The 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 the Quantitative Analysis Model pearl powder is proofreaied and correct and the 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, in conjunction with the method for qualitative analysis of similarity the matching analysis (Similarity Match Analysis), is set up the similarity coupling of pearl powder and is differentiated 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, foundation is for the quantitative discriminating model of pearl powder of doping oyster shell whiting, and realizes that with two models couplings application pearl powder mixes pseudo-effectively differentiating fast: the pseudo-pearl powder of mixing of differentiating the general impurity of doping by the similarity the matching analysis; By quantitative test, differentiate the pseudo-pearl powder of mixing of doping oyster shell whiting.Below modeling method and application thereof are illustrated.
Choose 10 batches, the pure pearl powder sample of fine qualities that comes from Zhejiang Province's Zhuji City, number consecutively is Z-1 to Z-10; 4 batches, pure mother-of-pearl shell powder, number consecutively is B-1 to B-4.Before sample carries out the near infrared spectrum test, in baking oven under 50 ℃ dry 12h to reduce the impact of moisture on test; With the abundant ground sample of agate mortar, reunite on the impact of test to reduce sample.
Use the FT-NIR Analyzer of instrument as the model Antaris II of Thermo Scientific company, spectral analysis software is Thermo Scientific company's T Q Analyst 9.0.The spectra collection condition is: the integrating sphere diffuse reflectance accessory; Spectral range 4000-10000cm
-1Resolution 8cm
-1Scanning times 64 times; The decay of instrument Automatic Optimal empty door, gain is 2.
The foundation of similarity the matching analysis 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 collected specimens Z-1 to Z-10 successively.Use TQ Analyst 9.0 to set up similarity the matching analysis model, design parameter arranges as follows:
Analysis type (Analysis Type): selection sort (Classification), similarity coupling (Similarity Match);
Light path type (Pathlength Type): select multicomponent signal to proofread and 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) is selected second derivative (Second Derivative) pre-service (Process Standards),
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 proofreading and correct (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 in proportion with nano-calcium carbonate, natural ostreae testa pulverata respectively, as shown in table 1.The similarity analysis model set up of application is mixed pseudo-sample to above-mentioned simulation and is analyzed, and result (in Table 1) shows that this model can differentiate the pearl powder of general impurity doping fast.
Table 1
Mix pseudo-pearl powder and quantitatively differentiate the foundation of model: choose each four, pearl powder sample and oyster shell whiting sample, accurately take pearl powder and oyster shell whiting mixes, and control the biased sample gross mass at 5g, biased sample fully grinds to be measured to mix with the agate grinding.Be specially that pearl powder Z-1 and oyster shell whiting B-1 adulterate mutually, pearl powder Z-2 and oyster shell whiting B-2 adulterates mutually, pearl powder Z-3 and oyster shell whiting B-3 adulterate mutually, obtain a series of simulations 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; Pearl powder Z-4 and oyster shell whiting B-4 are adulterated mutually, obtain a series of simulations 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 acquisition correction collection sample successively; Choose testing sample V-1 to V-4 as the checking collection, gather near infrared spectrum according to the same terms.Use TQ Analyst 9.0 softwares 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 Least Squares, PLS);
Light path type (Pathlength Type): select multicomponent signal to proofread and correct (Multiplicative Signal Correction, MSC);
Component (Components): definition " pearl powder content " is Component, and Unit is " % ";
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) is selected 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 proofreading and correct (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, the checking collection) as shown in Figure 3, the calibration set related coefficient is 0.9999, proofreading and correct 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 the cross validation result, and related coefficient is 0.9903.Checking concentrate mix in pseudo-pearl powder and pure pearl powder that the pearl powder massfraction predicts the outcome (in Table 3) and the actual computation value between deviation less (<5%), institute's established model can quick and precisely be predicted the massfraction of mixing pearl powder in pseudo-pearl powder of doping oyster shell whiting, and differentiates surveyed pearl powder purity and quality with this.
Table 3
Above embodiment is described the preferred embodiment of the present invention; not scope of the present invention is limited; design under the prerequisite of spirit not breaking away from the present invention; various distortion and improvement that the common engineering technical personnel in this area make technical scheme of the present invention, all should fall in the definite protection domain of claims of the present invention.
Claims (8)
1. pearl powder is mixed pseudo-near infrared spectrum identification method, it is characterized in that applying the Fourier transform near infrared diffuse reflectance spectroscopy analytical technology and differentiates and generally mix pseudo-pearl powder in conjunction with the qualitative analysis model of similarity the matching analysis foundation.
2. pearl powder according to claim 1 is mixed pseudo-near infrared spectrum identification method, it is characterized in that applying the Fourier transform near infrared diffuse reflectance spectroscopy analytical technology and with discriminating, mixes pseudo-pearl powder in conjunction with the massfraction of pearl powder in the pearl powder of the Quantitative Analysis Model quantitative measurement doping oyster shell whiting of partial least square method foundation.
3. pearl powder according to claim 2 is mixed pseudo-near infrared spectrum identification method, it is characterized in that:
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, the spectra collection condition comprises: the integrating sphere diffuse reflectance accessory; Spectral range 4000-10000cm
-1
In the foundation of similarity the matching analysis model, choose at least 10 pure pearl powder samples as calibration set, use near infrared spectrum software to set up similarity the matching analysis model: light path type selecting multicomponent signal is proofreaied and correct; Second derivative is adopted in the spectrum pre-service; The filtering of level and smooth employing Norris derivative; SPECTRAL REGION is at 4000-10000cm
-1In scope;
Mixing pseudo-pearl powder massfraction quantitatively differentiates in the foundation of model and to adopt pure pearl powder and the mode that pure oyster shell whiting mixes mutually to simulate the pseudo-pearl powder of mixing of doping oyster shell whiting, accurately take pearl powder and oyster shell whiting mixes, and control the biased sample gross mass more than 5g, using the qualitative characteristics quantitative parameter of the massfraction of pearl powder in biased sample as biased sample, the pearl powder massfraction of doped samples is calculated by doping ratio, simultaneously pure pearl powder massfraction is defined as to 100%, 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, use partial least square method to set up Quantitative Analysis Model: light path type selecting multicomponent signal is proofreaied and correct, second derivative is adopted in the spectrum pre-service, the filtering of level and smooth employing Norris derivative, SPECTRAL REGION is at 4000-10000cm
-1in scope.
4. pearl powder according to claim 3 is mixed pseudo-near infrared spectrum identification method, it is characterized in that, sample carries out carrying out drying and fully grinding before the near infrared spectrum test.
5. pearl powder according to claim 4 is mixed pseudo-near infrared spectrum identification method, it is characterized in that, in baking oven under 50 ℃ dry 12h to reduce the impact of moisture on test; With the abundant ground sample of agate mortar, reunite on the impact of test to reduce sample.
6. pearl powder according to claim 4 is mixed pseudo-near infrared spectrum identification method, it is characterized in that, the spectra collection condition also comprises: resolution 8cm
-1Scanning times 64 times; Use the gain parameter of instrument Automatic Optimal.
7. be used to differentiating that pearl powder mixes the method for building up of pseudo-analytical model, 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 the similarity the matching 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, the spectra collection condition comprises: the integrating sphere diffuse reflectance accessory; Spectral range 4000-10000cm
-1
In the foundation of similarity the matching analysis model, choose at least 10 pure pearl powder samples as calibration set, use near infrared spectrum software to set up similarity the matching analysis model: light path type selecting multicomponent signal is proofreaied and correct; Second derivative is adopted in the spectrum pre-service; The filtering of level and smooth employing Norris derivative; SPECTRAL REGION is at 4000-10000cm
-1In scope;
Mixing pseudo-pearl powder massfraction quantitatively differentiates in the foundation of model and to adopt pure pearl powder and the mode that pure oyster shell whiting mixes mutually to simulate the pseudo-pearl powder of mixing of doping oyster shell whiting, accurately take pearl powder and oyster shell whiting mixes by a certain percentage, and control the biased sample gross mass more than 5g, using the qualitative characteristics quantitative parameter of the massfraction of pearl powder in biased sample as biased sample, the pearl powder massfraction of doped samples is calculated by doping ratio, simultaneously pure pearl powder massfraction is defined as to 100%, 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, use partial least square method to set up Quantitative Analysis Model: light path type selecting multicomponent signal is proofreaied and correct, second derivative is adopted in the spectrum pre-service, the filtering of level and smooth employing Norris derivative, SPECTRAL REGION is at 4000-10000cm
-1in scope.
8. the analytical model of method foundation claimed in claim 7 is mixed pseudo-purposes for differentiating pearl powder.
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| CN103698281A (en) * | 2013-12-31 | 2014-04-02 | 四川新绿色药业科技发展股份有限公司 | Fructus psoraleae and near-infrared diffuse reflection measurement method of fructus psoraleae derivative |
| CN103837492A (en) * | 2014-02-24 | 2014-06-04 | 西北农林科技大学 | Nondestructive detection method for swelled kiwi fruits based on near-infrared spectrum technology |
| 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 |
| CN111337448A (en) * | 2020-03-26 | 2020-06-26 | 杭州老爸标准技术集团有限公司 | Method for identifying cosmetics based on infrared spectrum technology |
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| CN111337448A (en) * | 2020-03-26 | 2020-06-26 | 杭州老爸标准技术集团有限公司 | Method for identifying cosmetics based on infrared spectrum technology |
| 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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