CN108802003B - Method for rapidly and nondestructively identifying silk product and content - Google Patents
Method for rapidly and nondestructively identifying silk product and content Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000001237 Raman spectrum Methods 0.000 claims abstract description 30
- 238000001069 Raman spectroscopy Methods 0.000 claims abstract description 28
- 238000001228 spectrum Methods 0.000 claims abstract description 14
- 239000004744 fabric Substances 0.000 claims abstract description 10
- 230000000007 visual effect Effects 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 5
- 239000000835 fiber Substances 0.000 claims description 27
- 108010022355 Fibroins Proteins 0.000 claims description 17
- 239000000126 substance Substances 0.000 claims description 13
- 238000004364 calculation method Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- ZZIZZTHXZRDOFM-XFULWGLBSA-N tamsulosin hydrochloride Chemical compound [H+].[Cl-].CCOC1=CC=CC=C1OCCN[C@H](C)CC1=CC=C(OC)C(S(N)(=O)=O)=C1 ZZIZZTHXZRDOFM-XFULWGLBSA-N 0.000 claims description 3
- 241000255789 Bombyx mori Species 0.000 claims description 2
- 238000011002 quantification Methods 0.000 claims description 2
- 238000012360 testing method Methods 0.000 claims description 2
- 230000001066 destructive effect Effects 0.000 claims 3
- 238000004458 analytical method Methods 0.000 abstract description 4
- 238000003384 imaging method Methods 0.000 abstract description 3
- 238000004445 quantitative analysis Methods 0.000 abstract description 2
- 108090000623 proteins and genes Proteins 0.000 description 4
- 102000004169 proteins and genes Human genes 0.000 description 4
- 229920002994 synthetic fiber Polymers 0.000 description 4
- 239000012209 synthetic fiber Substances 0.000 description 4
- 229920000742 Cotton Polymers 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- 229920001223 polyethylene glycol Polymers 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- 229920001661 Chitosan Polymers 0.000 description 2
- 238000009841 combustion method Methods 0.000 description 2
- 238000007405 data analysis Methods 0.000 description 2
- 229920002620 polyvinyl fluoride Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000004451 qualitative analysis Methods 0.000 description 2
- 229920006052 Chinlon® Polymers 0.000 description 1
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- 150000001875 compounds Chemical class 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
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Abstract
The invention discloses a method for rapidly and nondestructively identifying silk products and content. The invention comprises the following steps: carrying out single-point scanning or imaging scanning on the quasi-appraised object by using a visual laser Raman spectrometer to obtain a single Raman spectrum or a series of Raman spectra; and comparing the standard spectrum of the silk to identify whether the quasi-appraisal object is a silk product, analyzing the content of the silk in the quasi-appraisal object, and applying the modern technological means to the identification of silk products such as silk fabrics, silk cultural relics, silk materials, silk artworks and the like. The method for identifying the silk product not only can realize traceless, lossless, simple and rapid identification of the silk product, but also can carry out quantitative analysis on the silk product, so that the method provides more choices for identification and analysis of the silk product, and has wide application prospect.
Description
Technical Field
The invention belongs to the technical field of biology, and particularly relates to a method for rapidly and nondestructively identifying silk products and content.
Background
Silk has important applications in the fields of food, chemical industry, biomedicine, etc., in addition to being used as a raw material of silk clothes in the textile industry. Since the price of the fibroin is higher than that of other natural or synthetic fibers, illegal vendors often mix other natural fibers (such as cotton and the like) or synthetic fibers (such as terylene, chinlon and the like) or sell the natural fibers or the synthetic fibers as the silk fibers, so that the market order is seriously disturbed, and the rights and interests of consumers are infringed. Furthermore, archaeological sites often have unearthed textile residues that need to be characterized and quantified. How to quickly, nondestructively, simply identify and quantify textile residues is receiving increasing attention and research in archaeological studies. Therefore, the method for carrying out specificity identification on the silk product has great application prospect.
Common methods for identifying silk products include combustion method, high performance liquid chromatography, infrared spectroscopy identification method and the like. The combustion method is a widely known method for identifying silk fibers, but the method has the disadvantages of poor specificity and high requirements for personnel, thereby having great misjudgment and loss of silk fibers. The high performance liquid chromatography is to dissolve silk fiber into aqueous solution in high concentration salt ion, and then identify the molecular weight of the silk solution by a high performance liquid chromatograph. The infrared spectrum identification method has the defects of poor specificity, sample damage and complex operation like the high performance liquid chromatography. In summary, there is no simple, rapid and nondestructive method for identifying and quantifying silk products or silk materials.
Disclosure of Invention
In order to solve the problems in the background technology, the invention provides a method for rapidly and nondestructively identifying silk products and content, which takes silk materials as target objects, and uses a commercial visual laser Raman spectrometer to carry out single-point scanning or imaging scanning on the target objects without any treatment to obtain a single or a series of Raman spectra; and comparing with a standard map, thereby identifying whether the quasi-identifier is a silk product.
The technical scheme adopted by the invention is as follows:
the method for rapidly and nondestructively identifying the silk product and the content comprises the following steps:
1) carrying out single-point scanning or imaging scanning on the quasi-appraised object by using a visual laser Raman spectrometer to obtain a single Raman spectrum or a series of Raman spectra;
2) comparing the Raman spectrum obtained in the step 2) with the silk standard spectrum to identify whether the quasi-identification substance is a silk product.
The peak value range of the silk standard map in the step 2) contains 3058-3062cm-1、2932-2936cm-1、2875-2880cm-1、1662-1668cm-1、1446-1452cm-1、1228-1231cm-1、1081-1086cm-1、851-855cm-1Wherein the peak value range of the strong characteristic peak is 3058-3062cm-1、1662-1668cm-1、1446-1452cm-1、1228-1231cm-1、1081-1086cm-1(ii) a At least four peak values in different peak value ranges of the silk standard map appear in the Raman map obtained in the step 1), or at least three peak values in different strong characteristic peak value ranges of the silk standard map appear in the Raman map, and the peak type characteristics of the quasi-identifier are similar to those of the silk standard map, namely the quasi-identifier is judged to be a silk product or a silk-containing raw material。
The scanning parameters during scanning comprise laser power, exposure time, scanning times, pixels and total scanning time.
The scanning parameters during scanning are set as follows: laser power is 1-8mW, exposure time is 1-100Hz, scanning times are 1-300 times, and pixels are 0.2-2 μm.
And (3) comparing the Raman spectrum of the quasi-identifier obtained in the step 2) with the silk standard spectrum obtained in the step 1) and reducing and determining the content of silk in the quasi-identifier.
The silk standard spectrum in the step 2) is obtained by reeling silk on the spun silkworm cocoons to obtain silk fibers, and placing the silk fibers in a Raman spectrometer for testing.
The quasi-identification object in the step 2) comprises silk fabrics, silk cultural relics, silk materials and silk artworks.
The principle of the visual laser Raman spectrometer is that incident laser can cause molecules of a substance to be detected to vibrate, so that the frequency of scattered light changes, and the analysis of the scattered light is Raman spectrum analysis. Due to the uniqueness of the components of the fibroin molecules, the silk product can be rapidly, in-situ, repeatedly and nondestructively detected by a visual laser Raman spectrometer (such as a laser confocal Raman spectrometer), and effective information such as components, structures, relative contents and the like of the silk molecules can be detected, so that the aim of simply, rapidly and nondestructively identifying the silk product is fulfilled.
The invention has the beneficial effects that:
1) and (3) fast: according to the invention, no pretreatment is needed to be carried out on the sample, the spectrogram can be obtained in about 0.5 minute, and the complex data analysis on the obtained result is not needed;
2) lossless: the invention does not need to process the sample, does not damage the original sample, and can directly put the sample into the Raman spectrometer for single-point detection;
3) the specificity is strong: the Raman spectrum of the silk fiber obtained by the invention is obviously different from the Raman spectra of other natural or synthetic fibers;
4) the sensitivity is high: the selected sample can be a macroscopic silk product or a micron-sized silk product, and can be identified;
5) and (3) qualitative analysis: the method can be used for accurately and qualitatively analyzing the substance to be detected mixed with the fibroin and can also be used for carrying out in-situ analysis on the substance to be detected so as to accurately measure the content and distribution of the fibroin in the substance to be detected.
Drawings
FIG. 1 is a standard spectrum of silk of example 1;
FIG. 2 shows a comparison of the spectra of the silk product of example 2 with other fibers;
FIG. 3 is a graph of silk products of different forms in example 3;
fig. 4 is a graph showing the in-situ distribution and content of fibroin in the composite silk product of example 4.
Detailed Description
The present invention is further illustrated by the following examples, which are illustrative of the present invention and are not to be construed as being limited thereto.
The examples of the invention are as follows:
example 1:
(1) and carrying out single-point scanning on the silk fiber standard product by using a visual laser Raman spectrometer to obtain a Raman spectrum of the silk protein standard product. Scanning parameter setting: laser power 1mW, exposure time 10Hz, scanning times 100 times, pixel 0.5 μm, total scanning time 20 seconds.
(2) And (3) smoothing, baseline adjustment and peak marking are carried out on the Raman spectrum obtained in the step (1), so that all peak values and strong characteristic peaks of the fibroin standard product are obtained. As shown in figure 1, the peak value of the silk standard map contains 3058-3062cm-1、2932-2936cm-1、2875-2880cm-1、1662-1668cm-1、1446-1452cm-1、1228-1231cm-1、1082-1086cm-1、851-855cm-1Equipeak value, wherein the strong characteristic peak is 3058-3062cm-1、1662-1668cm-1、1446-1452cm-1、1228-1231cm-1、1082-1086cm-1。
(3) And carrying out single-point scanning on the silk fabric to-be-detected product by using a visual laser Raman spectrometer to obtain a Raman spectrum of the silk fabric to-be-detected product. Scanning parameter setting: laser power 8mW, exposure time 100Hz, scanning times 1, pixel 2 μm, total scanning time about 5 seconds.
(4) And (3) comparing the Raman spectrum obtained in the step (1) with the silk standard spectrum without carrying out complex data analysis, thereby identifying whether the quasi-identification substance is a silk product. As shown in fig. 2, when multiple fabrics such as polyvinyl fluoride fibers, chitosan fibers and cotton fibers are identified, the peak value, peak height, peak width and peak area in the silk standard map are different from those of multiple fabrics such as polyvinyl fluoride fibers, chitosan fibers and cotton fibers, so that the silk fabric can be distinguished from other silk fabrics.
Example 2:
the above steps (1) and (2) of example 1 were used.
(3) And performing single-point scanning on silk products such as silk protein fibers, silk fabrics, silk fibroin powder and the like by using a visual laser Raman spectrometer to obtain a Raman spectrum of the fiber to-be-detected product.
Scanning parameter setting: laser power 4mW, exposure time 1Hz, scanning times 300 times, pixel 0.2 μm, total scanning time about 30 seconds.
(4) And (2) comparing the Raman spectrums obtained in the step (1). As shown in fig. 3: the characteristic peak values, peak heights, peak widths and peak areas of the silk protein fibers, the silk products and the silk fibroin powder are all similar, so that the Raman spectra of the silk protein in different states are consistent and have the same molecular consistency.
Example 3:
the above steps (1) and (2) of example 1 were used.
(3) And (3) carrying out in-situ surface scanning on the fiber to-be-detected product by using a visual laser confocal Raman spectrometer to obtain a Raman two-dimensional image of the fiber to-be-detected product in a certain area (manually selected). Scanning parameter setting: laser power 4mW, exposure time 5Hz, scanning times 50 times, pixel 1.5 μm, total scanning time 30 minutes.
(4) Comparing and reducing the Raman two-dimensional image in the step (1) with a silk standard spectrum, rapidly determining the silk content and the silk distribution in the fiber to-be-detected product through MCR of a Raman spectrometer, and finding that the fiber to-be-detected product has an obvious fibroin Raman peak spectrum and polyethylene glycol (PEG) Raman peak spectrum. The fibroin is uniformly distributed in the fiber product to be detected, and accounts for 79.2% of the fiber product to be detected, the PEG accounts for 14.3% of the fiber product to be detected, and the balance is other substances.
Compared with the traditional Raman spectrometer, the confocal laser Raman spectrometer has a confocal imaging function and is integrated with OMNIC Atl mu s image processing software, and can map the spectrum with micron-level resolution and integrate an image analysis algorithm and a chemical metering tool together.
The MCR process of this example is: firstly, a selected area of a silk fibroin sample is imaged by using a confocal laser Raman spectrometer, a laser scanning beam is used for forming a point light source through a grating pinhole, point-by-point scanning is carried out on a focal plane, and a high-definition and high-resolution nanoscale multipoint Raman spectrum is obtained, wherein one point represents a peak value; and then, performing second derivative calculation on each Raman spectrum peak value by using OMNIC Atl mu s image software, dividing the Raman spectrum peak value into a plurality of peaks, performing calculation according to the peak values to finish the quantification of one Raman spectrum, and obtaining the quantitative information of all the fibroin-containing substances after all the Raman spectrums in a specific area are scanned.
According to the identification results of the embodiments 1, 2 and 3, whether the different substances to be detected are the fibroin can be accurately identified by using the laser raman spectroscopy technology provided by the application. According to the analysis result of the embodiment 4, the distribution and the content of the fibroin in the compound can be accurately identified by using the laser raman spectroscopy technology provided by the application, and the resolution is very high. Therefore, the method for rapidly and nondestructively identifying the silk product and the content can accurately perform qualitative analysis on the existence of the fibroin in the object to be detected and also can perform quantitative analysis on the silk in the object to be detected, and has the advantages of rapidness, simplicity, nondestructiveness, high efficiency and repeatability.
Claims (4)
1. A method for rapidly and nondestructively identifying silk products and content is characterized by comprising the following steps:
1) performing single-point scanning on the quasi-appraisal object by using a visual laser Raman spectrometer to obtain a single or a series of Raman spectrums;
2) comparing the Raman spectrum obtained in the step 1) with a silk standard spectrum to identify whether the quasi-identification substance is a silk product;
the peak value range of the silk standard map in the step 2) contains 3058-3062cm-1、2932-2936cm-1、2875-2880cm-1、1662-1668cm-1、1446-1452cm-1、1228-1231cm-1、1081-1086cm-1、851-855cm-1Wherein the range of the strong characteristic peak is 3058-3062cm-1、1662-1668cm-1、1446-1452cm-1、1228-1231cm-1、1081-1086cm-1(ii) a If at least four peak values in different peak value ranges of the silk standard map or at least three peak values in different strong characteristic peak value ranges of the silk standard map appear in the Raman map obtained in the step 1), judging that the quasi-identification object is a silk product or a silk-containing raw material;
comparing the Raman spectrum of the quasi-identifier with the silk standard spectrum and reducing and determining the content of silk in the quasi-identifier; firstly, a selected area of a silk fibroin sample is imaged by using a confocal laser Raman spectrometer, a laser scanning beam is used for forming a point light source through a grating pinhole, point-by-point scanning is carried out on a focal plane, and a high-definition and high-resolution nanoscale multipoint Raman spectrum is obtained, wherein one point represents a peak value; and then, performing second derivative calculation on each Raman spectrum peak value by using OMNIC Atl mu s image software, dividing the Raman spectrum peak value into a plurality of peaks, performing calculation according to the peak values to finish the quantification of one Raman spectrum, and obtaining the quantitative information of all the fibroin-containing substances after all the Raman spectrums in a specific area are scanned.
2. The method for rapid and non-destructive identification of silk products and silk content as claimed in claim 1, wherein: the silk standard spectrum in the step 2) is obtained by reeling silk on the spun silkworm cocoons to obtain silk fibers, and placing the silk fibers in a Raman spectrometer for testing.
3. The method for rapid and non-destructive identification of silk products and silk content as claimed in claim 1, wherein: the scanning parameters during scanning are set as follows: laser power is 1-8mW, exposure time is 1-100Hz, scanning times are 1-300 times, and pixels are 0.2-2 μm.
4. The method for rapid and non-destructive identification of silk products and silk content as claimed in claim 1, wherein: the quasi-identification object in the step 2) comprises silk fabrics, silk cultural relics, silk materials and silk artworks.
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| JPH06273334A (en) * | 1993-03-24 | 1994-09-30 | Densen Sogo Gijutsu Center | Nondestructive deterioration diagnostic method for polyolefin molded item |
| CN101285773A (en) * | 2008-05-23 | 2008-10-15 | 浙江大学 | Blended fabric component Raman spectra qualitative checking method |
| CN104122250A (en) * | 2014-07-04 | 2014-10-29 | 华东理工大学 | Method for rapid detection of lactose in milk |
| CN104359889A (en) * | 2014-10-27 | 2015-02-18 | 徐敦明 | Method for quickly and nondestructively distinguishing between real and fake bird's nests |
| CN104749158A (en) * | 2013-12-27 | 2015-07-01 | 同方威视技术股份有限公司 | Jade jewelry appraisal method and device thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06273334A (en) * | 1993-03-24 | 1994-09-30 | Densen Sogo Gijutsu Center | Nondestructive deterioration diagnostic method for polyolefin molded item |
| CN101285773A (en) * | 2008-05-23 | 2008-10-15 | 浙江大学 | Blended fabric component Raman spectra qualitative checking method |
| CN104749158A (en) * | 2013-12-27 | 2015-07-01 | 同方威视技术股份有限公司 | Jade jewelry appraisal method and device thereof |
| CN104122250A (en) * | 2014-07-04 | 2014-10-29 | 华东理工大学 | Method for rapid detection of lactose in milk |
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