CN105486656A - Method for detecting content of acid orange added in chilli powder - Google Patents

Method for detecting content of acid orange added in chilli powder Download PDF

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Publication number
CN105486656A
CN105486656A CN201510851487.9A CN201510851487A CN105486656A CN 105486656 A CN105486656 A CN 105486656A CN 201510851487 A CN201510851487 A CN 201510851487A CN 105486656 A CN105486656 A CN 105486656A
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acid orange
content
chilli powder
absorbance
linear regression
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CN201510851487.9A
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Chinese (zh)
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李晓丽
张裕莹
何勇
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Zhejiang University ZJU
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Zhejiang University ZJU
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3563Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor

Abstract

The invention discloses a method for detecting content of acid orange added in chilli powder. The method comprises the following steps: (1) chilli powder with different contents of acid orange are used as test samples, and infrared absorption spectrum of each test sample in a set wave range is obtained; (2) according to the infrared absorption spectrum of the test sample, transmissivity of characteristic absorption peak of acid orange is extracted, and absorbance of each characteristic absorption peak is obtained; (3) a linear regression model between the acid orange content and each absorbance is established; (4) absorbance of a sample to be measured at the characteristic absorption peak of acid orange is obtained, and according to the linear regression model, the content of acid orange in the sample to be measured is obtained by calculation. The method has the advantages of simplicity, rapid and high accuracy.

Description

In a kind of chilli powder, acid orange adds the detection method of content
Technical field
The present invention relates to the detection of acid orange content, particularly relate to acid orange in a kind of chilli powder and add the detection method of content.
Background technology
Acid Orange II has another name called acid golden yellow II, gold orange II or acid gorgeous orange GR, and popular name Acid orange Ⅱ, is a kind of azo Prof. Du Yucang dyestuff, is mainly used in the dyeing of textile, leather and fur products, plastics and woodwork, has strong carcinogenicity.China's clear stipulaties, Acid Orange II is non-edible material from soybeans, forbids adding in food using.But because it has lovely luster, good level-dyeing property, lower-price characteristic, production and the processing of capsicum and goods thereof is often used for by illegal businessman, bring great hidden danger to the food security of people, therefore, be necessary the method setting up Acid Orange II in a kind of quick detection capsicum and goods thereof.
At present, high performance liquid chromatography, thin-layered chromatography, fluorescent spectrometry and Liquid Chromatography/Mass Spectrometry is had to the assay method of Acid Orange II in the food such as bean product, meat products, fruit juice.But Acid Orange II mensuration report is still rare in chilli products.
High performance liquid chromatography is a chromatographic important branch, take liquid as mobile phase, adopt high pressure transfusion system, the mobile phase such as mixed solvent, damping fluid of the single solvent or different proportion with opposed polarity is pumped into the chromatographic column that Stationary liquid is housed, in post each composition separated after, enter detecting device to detect, thus realize the analysis to sample.The advantage of the method is that separation efficiency is high, and selectivity is good, and detection sensitivity is high, operation automation, applied range, but analysis cost is high, does not have abundant experiment experience to be difficult to once complete detection.
Thin-layered chromatography (TLC) is coated on glass plate, plastics or aluminium substrate by suitable Stationary liquid, becomes a thin uniform layer.Until point sample, launch after, the Rf value (Rf) according to Rf value (Rf) and the suitable tester chromatogram of gained by the same method compares, in order to carry out the method for assay.The method is simple to operate, and colour developing is convenient, but the poor reproducibility of the method.
The principle of atomic fluorescence spectrometry (AFS) is that atomic vapour absorbs the optical radiation of certain wavelength and is excited, excited atom launches the optical radiation of certain wavelength subsequently by excitation process, under certain experiment condition, its radiation intensity is directly proportional to atom content.The features such as atomic fluorescence spectrometry has highly sensitive, and selectivity is strong, and the few and method of sample size is simple; But it is extensive not enough that its weak point is range of application.
LC-MS (HPLC-MS) be LC-MS-MS again, and it is using liquid chromatography as piece-rate system, and mass spectrum is detection system.Sample is separated with mobile phase in mass spectrum part, and after being ionized, separated by mass number by fragment ion through mass spectrographic mass analyzer, device obtains mass spectrogram after testing.LC-MS embodies the complementation of chromatogram and mass spectrum advantage, by the high separating power of chromatogram to complex sample, with MS, there is high selectivity, high sensitivity and the advantages of relative molecular mass and structural information can be provided, but it is difficult to the structural information obtaining material, main dependence and reference material contrast to judge unknown material, also will be analyzed by other approach the detection without ultraviolet absorption compound.
Above method all needs to add various chemical reagent and then from sample, isolate determinand to detect, but operation steps more complicated in analytic process, and influence factor is more, so accurately cannot determine that the material detected necessarily derives from former state originally.And need to use a large amount of reagent when detecting in order to upper method and carry out pre-treatment, process is loaded down with trivial details, cannot accomplish quick detection.
Summary of the invention
Acid orange in a kind of chilli powder is the object of the present invention is to provide to add the detection method of content, the advantage that the method has simply, quick, accuracy is high.。
For achieving the above object, the invention provides following technical scheme:
In chilli powder, acid orange adds a detection method for content, comprising:
(1) using the chilli powder of different acid orange content as test sample book, the infrared absorption spectrum of each test sample book in setting wave-number range is obtained;
(2) according to the infrared absorption spectrum of test sample book, extract the transmissivity of the characteristic absorption peak of acid orange, obtain the absorbance of each characteristic absorption peak;
(3) linear regression model (LRM) between acid orange content and each absorbance is set up;
(4) obtain the absorbance of sample to be tested at the characteristic absorption peak place of acid orange, according to described linear regression model (LRM), calculate the content of acid orange in testing sample.
Infra-red sepectrometry is in fact a kind of analytical approach determining material molecular structure and discriminating compound according to information such as the interatomic Relative Vibration of intramolecule and molecule rotation.The various groups of ingredient have oneself specific infrared signature absorption peak, can realize accordingly " fingerprint verification " of some chemical bond and functional group in molecule.Infrared spectrum, as the means of testing of molecular level, is easy to the Components identification analysis realizing COMPLEX MIXED objects system.
Multiple linear regression analysis is used to dependence between research dependent variable and one group of independent variable, by extracting the absorbance at the infrared signature absorption peak place of acid orange, set up the linear regression model (LRM) between acid orange content and each absorbance, then bring each corresponding absorbance of testing sample into content that linear regression model (LRM) just can draw the acid orange in sample to be tested.
This detection method step is few, simple to operate, avoids the Sample Preparation Procedure that classic method is loaded down with trivial details, consuming time, achieves Aulomatizeted Detect, and speed is fast, and precision is high; And Sample Preparation Procedure can not consume a large amount of chemical reagent as traditional detection, therefore can not cause adverse effect to environment, environmental protection.
In step (1), by chilli powder, as detected object, each detected object and acid orange are mixed according to a certain ratio, prepare the test sample book of one group of acid orange content distribution gradient.
Infrared spectrum separately through a certain test sample book is difficult to the characteristic absorption peak determining acid orange accurately, by carrying out statistical analysis to large sample in the present invention, can find out the characteristic absorption peak of acid orange accurately.Usual sample size is more, and it is more accurate that characteristic absorption peak judges, but calculated amount can be caused so large, and efficiency is low.Therefore the number needs of test sample book will be considered according to actual conditions, can not be too high, can not be too low.In addition, can be divided into some groups (being generally 5 ~ 7 groups) for ease of realizing all test sample books, the acid orange content of each group is identical, and the acid orange content between different groups carries out gradient setting.
As preferably, the quantity of test sample book is 50 ~ 100; More preferably 100.
Obtain the infrared absorption spectrum of each test sample book in setting wave-number range, as preferably, setting wave-number range is 400 ~ 4000cm -1, in chilli powder, the infrared signature absorption peak of acid orange is distributed in this wave-number range.
According to the infrared absorption spectrum of all test sample books, extract the characteristic absorption peak of acid orange, as preferably, the number of the characteristic absorption peak of the acid orange of extraction is 16.
As preferably, the characteristic absorption peak of the acid orange of extraction is respectively at 453cm -1, 461cm -1, 466cm -1, 489cm -1, 504cm -1, 516cm -1, 1533cm -1, 1582cm -1, 1797cm -1, 1967cm -1, 2428cm -1, 2433cm -1, 2437cm -1, 3562cm -1, 3767cm -1and 3874cm -1place.
In order to the convenience calculated, the transmissivity of each characteristic absorption peak is converted to absorbance, according to formula, transmissivity is converted to absorbance, described formula is:
A = log 1 T
Wherein, A is absorbance, and T is transmissivity.
By linear regression model (LRM) between the absorbance at acid orange content and each characteristic absorption peak place in test sample book, as preferably, multi-element linear regression method matching is adopted to set up linear regression model (LRM).
Described linear regression model (LRM) is:
Y=0.015345-0.0186λ 1+0.0159λ 2+0.0154λ 3+0.0225λ 4-0.0452λ 5+0.0265λ 6+0.25λ 7-0.205λ 8-0.0938λ 9-0.159λ 10+0.11λ 11-0.0859λ 12+0.102λ 13+0.143λ 14-0.28λ 15+0.233λ 16
Wherein, Y is acid orange content in chilli powder, and unit is mg/g; λ 1, λ 2, λ 3, λ 4, λ 5, λ 6, λ 7, λ 8, λ 9, λ 10, λ 11, λ 12, λ 13, λ 14, λ 15and λ 16be respectively 453cm -1, 461cm -1, 466cm -1, 489cm -1, 504cm -1, 516cm -1, 1533cm -1, 1582cm -1, 1797cm -1, 1967cm -1, 2428cm -1, 2433cm -1, 2437cm -1, 3562cm -1, 3767cm -1and 3874cm -1the absorbance at place.
Bring each corresponding absorbance of testing sample into content that linear regression model (LRM) just can draw the acid orange in sample to be tested.
Utilize the acid orange content of linear regression model (LRM) of the present invention to some samples to predict, the matching of unitary once linear is carried out, the related coefficient (R of this matched curve to the predicted value of each sample and actual value 2) reaching 0.940, root-mean-square error (RMSE) reaches 0.069, illustrates that linear regression model (LRM) of the present invention can realize effective detection of acid orange content in chilli powder.
Compared with prior art, beneficial effect of the present invention is:
(1) simple to operate, avoid the extraction of convention acidic orange content measurement, the Sample Preparation Procedure loaded down with trivial details, consuming time such as to clear up, in fast and effeciently Real-Time Monitoring chilli powder, the content of acid orange provides effective means, have a good application prospect;
(2) system architecture is simple, be easy to operation, and system maintenance is with low cost, substantially realizes Aulomatizeted Detect.
Accompanying drawing explanation
Fig. 1 is to the scatter diagram between the predicted value of acid orange content in sample and its actual value by linear regression model (LRM) of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
1, the foundation of linear regression model (LRM):
(1) chilli powder is mixed according to a certain ratio with acid orange, be mixed with the test sample book of acid orange content distribution gradient.
Take 0mg, 1mg, 2mg, 4mg, 8mg acid orange respectively, add 10g chilli powder respectively again, mix, obtain the mixed-powder of 0mg/g (acid orange quality/chilli powder quality), 0.1mg/g, 0.2mg/g, 0.4mg/g, 0.8mg/g ratio, be mixed with the detected object of 5 acid orange content distribution gradient.Each contents level gets 20 samples, and 5 detected objects totals obtain 100 test sample books.
By each test sample book and potassium bromide crystal (KBr) according to 1: 49 mass ratio mix, fully grind, compressing tablet.
(2) to the compressing tablet of each test sample book at 400 ~ 4000cm -1carry out infrared scan in wave-number range, obtain transmissivity, and according to formula, transmissivity (T) is converted to absorbance (A), formula is:
A = log 1 T
According to the absorbance of all test sample books, extract the wave number at 16 characteristic absorption peak places of acid orange, be respectively 453cm -1, 461cm -1, 466cm -1, 489cm -1, 504cm -1, 516cm -1, 1533cm -1, 1582cm -1, 1797cm -1, 1967cm -1, 2428cm -1, 2433cm -1, 2437cm -1, 3562cm -1, 3767cm -1and 3874cm -1.
(3) adopt polynary once linear regretional analysis to set up linear regression model (LRM) in chilli powder between acid orange content and the absorbance of each characteristic absorption peak, this linear regression model (LRM) is:
Y=0.015345-0.0186λ 1+0.0159λ 2+0.0154λ 3+0.0225λ 4-0.0452λ 5+0.0265λ 6+0.25λ 7-0.205λ 8-0.0938λ 9-0.159λ 10+0.11λ 11-0.0859λ 12+0.102λ 13+0.143λ 14-0.28λ 15+0.233λ 16
Wherein, Y is acid orange content in chilli powder, and unit is mg/g; λ 1, λ 2, λ 3, λ 4, λ 5, λ 6, λ 7, λ 8, λ 9, λ 10, λ 11, λ 12, λ 13, λ 14, λ 15and λ 16be respectively 453cm -1, 461cm -1, 466cm -1, 489cm -1, 504cm -1, 516cm -1, 1533cm -1, 1582cm -1, 1797cm -1, 1967cm -1, 2428cm -1, 2433cm -1, 2437cm -1, 3562cm -1, 3767cm -1and 3874cm -1the absorbance at place.
Obtain sample to be tested after the absorbance at the characteristic absorption peak place of acid orange, according to described linear regression model (LRM), the content of acid orange in testing sample can be calculated.
2, the inspection of linear regression model (LRM):
Utilize the compound method of test sample book, preparation acid orange content is respectively 5 groups of test samples of 0mg/g (acid orange quality/chilli powder quality), 0.1mg/g, 0.2mg/g, 0.4mg/g, 0.8mg/g, often group detects the sample number of sample is 20, amounts to 100 test samples.
The detection method of acid orange content in above-mentioned chilli powder is utilized to predict the content of acid orange in each test samples, and carry out the matching of unitary once linear by between the predicted value of acid orange content in each test samples and its actual value, the related coefficient (R of matched curve 2) reaching 0.940, root-mean-square error (RMSE) reaches 0.069, illustrates that linear regression model (LRM) of the present invention can realize effective detection of acid orange content in chilli powder.
Scatter diagram in test samples between the predicted value of acid orange content and its actual value as shown in Figure 1.

Claims (8)

1. in chilli powder, acid orange adds a detection method for content, it is characterized in that, comprising:
(1) using the chilli powder of different acid orange content as test sample book, the infrared absorption spectrum of each test sample book in setting wave-number range is obtained;
(2) according to the infrared absorption spectrum of test sample book, extract the transmissivity of the characteristic absorption peak of acid orange, obtain the absorbance of each characteristic absorption peak;
(3) linear regression model (LRM) between acid orange content and each absorbance is set up;
(4) obtain the absorbance of sample to be tested at the characteristic absorption peak place of acid orange, according to described linear regression model (LRM), calculate the content of acid orange in testing sample.
2. in chilli powder according to claim 1, acid orange adds the detection method of content, and it is characterized in that, setting wave-number range is 400 ~ 4000cm -1.
3. in chilli powder according to claim 1, acid orange adds the detection method of content, and it is characterized in that, the number of the characteristic absorption peak of the acid orange of extraction is 16.
4. in chilli powder according to claim 3, acid orange adds the detection method of content, and it is characterized in that, the characteristic absorption peak of the acid orange of extraction is respectively at 453cm -1, 461cm -1, 466cm -1, 489cm -1, 504cm -1, 516cm -1, 1533cm -1, 1582cm -1, 1797cm -1, 1967cm -1, 2428cm -1, 2433cm -1, 2437cm -1, 3562cm -1, 3767cm -1and 3874cm -1place.
5. in chilli powder according to claim 1, acid orange adds the detection method of content, it is characterized in that, adopts multi-element linear regression method matching to set up linear regression model (LRM).
6. in chilli powder according to claim 5, acid orange adds the detection method of content, and it is characterized in that, described linear regression model (LRM) is:
Y=0.015345-0.0186λ 1+0.0159λ 2+0.0154λ 3+0.0225λ 4-0.0452λ 5
+0.0265λ 6+0.25λ 7-0.205λ 8-0.0938λ 9-0.159λ 10+0.11λ 11
-0.0859λ 12+0.102λ 13+0.143λ 14-0.28λ 15+0.233λ 16
Wherein, Y is acid orange content in chilli powder, and unit is mg/g; λ 1, λ 2, λ 3, λ 4, λ 5, λ 6, λ 7, λ 8, λ 9, λ 10, λ 11, λ 12, λ 13, λ 14, λ 15and λ 16be respectively 453cm -1, 461cm -1, 466cm -1, 489cm -1, 504cm -1, 516cm -1, 1533cm -1, 1582cm -1, 1797cm -1, 1967cm -1, 2428cm -1, 2433cm -1, 2437cm -1, 3562cm -1, 3767cm -1and 3874cm -1the absorbance at place.
7. in chilli powder according to claim 1, acid orange adds the detection method of content, it is characterized in that, the method obtaining absorbance is: according to formula, transmissivity is converted to absorbance, described formula is:
Wherein, A is absorbance, and T is transmissivity.
8. in chilli powder according to claim 1, acid orange adds the detection method of content, and it is characterized in that, the quantity of test sample book is 50 ~ 100.
CN201510851487.9A 2015-11-27 2015-11-27 Method for detecting content of acid orange added in chilli powder Pending CN105486656A (en)

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Application publication date: 20160413