CN108693297A - A kind of method of TLC technique and Surface enhanced Raman spectroscopy technology combination detection synthetic food color - Google Patents
A kind of method of TLC technique and Surface enhanced Raman spectroscopy technology combination detection synthetic food color Download PDFInfo
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- CN108693297A CN108693297A CN201810510705.6A CN201810510705A CN108693297A CN 108693297 A CN108693297 A CN 108693297A CN 201810510705 A CN201810510705 A CN 201810510705A CN 108693297 A CN108693297 A CN 108693297A
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- enhanced raman
- raman spectroscopy
- nanorod array
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
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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
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
- G01N30/94—Development
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Abstract
The invention discloses a kind of methods of TLC technique and Surface enhanced Raman spectroscopy technology combination detection synthetic food color, include the following steps:A, the preparation of Silver nanorod array substrate:Titanium film and Ag films are deposited in glass substrate surface using glancing angle deposition technology, continues deposition of silver nanometer rods after adjusting deposition angles;B, Development of Thin-Layer Chromatography:Development of Thin-Layer Chromatography is carried out to the synthetic food color in Silver nanorod array substrate using methanol;C, Surface enhanced Raman spectroscopy detects:Raman spectrum detection is carried out to the sample after expansion.Different synthetic food colors can quickly be distinguished, have many advantages, such as that operating process is simple, at low cost, highly sensitive.
Description
Technical field
The present invention relates to a kind of TLC techniques and Surface enhanced Raman spectroscopy technology combination detection synthetic food color
Method, specifically, being to be related to a kind of Surface enhanced Raman scattering based on Silver nanorod array substrate and thin-layer chromatography exhibition
The detection method to synthetic food color associated with technology is opened, material technical field of food detection is belonged to.
Background technology
Currently, Surface enhanced Raman spectroscopy has become a powerful analysis tool, surface vibration spectrum is extended,
The solution of possibility is provided for a large amount of Chemical Problem.In reagent diagnosis, to some ideal surface-enhanced Ramans
Scattering substrate has higher requirement, such as:It is high to enhance performance, favorable repeatability, uniformity is strong, and the service life stablizes, and is simple to manufacture.
But surface enhanced Raman scattering substrate is usually required by complicated either physically or chemically formation, Er Qieduo
Number does not have reusable characteristic, so just there is the problem of resource and artificial waste, testing cost improves.
Invention content
For above-mentioned existing technical problem, the present invention provides a kind of simple and effective Silver nanorod array surface enhancing drawing
The preparation method of graceful scattering substrate, using TLC technique as quick pretreatment technology and Surface enhanced Raman scattering
Technology can be detached and be detected to synthetic food color as quick detection technique.
To achieve the above object, a kind of TLC technique of present invention offer is examined with the combination of Surface enhanced Raman spectroscopy technology
The method for surveying synthetic food color, includes the following steps:
A, the preparation of Silver nanorod array substrate:Using glancing angle deposition technology glass substrate surface deposition titanium film and
Ag films continue deposition of silver nanometer rods after adjusting deposition angles;
B, Development of Thin-Layer Chromatography:Thin-layer chromatography is carried out to the synthetic food color in Silver nanorod array substrate using methanol
Expansion;
C, Surface enhanced Raman spectroscopy detects:Raman spectrum detection is carried out to the sample after expansion.
Preferably, the preparation method of the Silver nanorod array substrate is as follows:By long 2.5cm, the glass substrate of wide 0.5cm
It is fixed on sample stage surface and is right against steam incident direction, be less than 10 in film deposition vacuum cavity air pressure-6When Torr, utilize
The titanium film of one layer of 20nm is deposited in glass substrate surface for electron beam deposition coating method, waits for that film deposition vacuum cavity is cooled to titanium
Continue to be deposited the Ag films of one layer of 100nm after coating materials solidification to form bottom surface enhancing Raman scattering structure, waits for that cavity cools down
After being solidified to silverskin material, make sample stage normal with steam incident direction in 85 °, continues to be deposited 2000nm Ag films to form upper layer
Surface enhanced Raman scattering Silver nanorod array structure.
Preferably, the Development of Thin-Layer Chromatography method is as follows:In a long 2cm, wide 2cm, in the quartz colorimetric utensil of high 3cm
600 μ L absolute methanols are added;Be placed on cuvette mouth using a piece of clean glass slide, wait for 1min make in cuvette without water beetle
Alcohol atmosphere is saturated;On Silver nanorod array substrate surface from 2 μ L synthetic food colors of dropwise addition at the bottom 0.5cm of nanowire growth direction
Sample, at the center of dropwise addition origin is unfolded to mark in work after air-drying;Silver nanorod array substrate oblique cutting is entered into quartz colorimetric utensil
In, it is 70 °~75 ° to have the face-up of sample, angle, covers glass slide, makes absolute methanol band in Silver nanorod array substrate
Coloring vegetarian refreshments is freely unfolded;After absolute methanol can not continue expansion, it is to be detected to take out Silver nanorod array substrate natural air drying.
Preferably, the Raman spectrum method for detecting surface reinforcement is as follows:Substrate is placed under Raman spectrometer probe, is swept
Face initial point is that sample origin is added dropwise, and scans 5 random points every 1mm along expansion direction, is carried out to the characteristic peak in spectrum
Analysis.
Preferably, glass substrate is fixed on by sample stage surface using Teflon adhesive tape.
Preferably, the sample stage is using round stainless steel sample stage.
Advantages of the present invention:Different synthetic food colors can quickly be distinguished, have operating process it is simple, at
The advantages that this is low, highly sensitive.
Description of the drawings
Fig. 1 is that result figure is unfolded in the synthetic food color of the embodiment of the present invention 1;
Fig. 2 is the Surface enhanced Raman spectroscopy of the synthetic food color of present example 1.
Specific implementation mode
The invention will be further described below in conjunction with the accompanying drawings, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment:The thin-layer chromatography of six kinds of synthetic food colors-Surface enhanced Raman spectroscopy technology combination, concrete operations step
It is rapid as follows.
1, by long 2.5cm, the glass substrate of wide 0.5cm is fixed on sample stage surface face using heat-resisting Teflon adhesive tape
In steam incident direction, it is less than 10 in cavity air pressure-6When Torr, the titanium that one layer of 20nm is deposited using electron beam deposition coating method is thin
For film so that surface texture has good adhesive with glass substrate, the silver for continuing one layer of 100nm of vapor deposition after cavity cooling is thin
Film enhances Raman scattering structure to form bottom surface, after cavity cooling, makes the sample stage normal be in steam incident direction
85 °, continues to be deposited 2000nm Ag films to form upper surface enhancing Raman scattering Silver nanorod array structure, finally obtain silver
Nanometer stick array substrate.
2, in a long 2cm, wide 2cm is added 600 μ L absolute methanols in the quartz colorimetric utensil of high 3cm, and absolute methanol sheet
Body is without Surface-Enhanced Raman Scattering Characteristics peak and is easy to be unfolded in Silver nanorod array substrate;Use a piece of clean glass slide
It is placed on cuvette mouth, waits for 1min that the methanol atmosphere in cuvette is made to be saturated;It is given birth to from nanometer on Silver nanorod array substrate surface
2 μ L synthetic food color samples are added dropwise at the 0.5cm of length direction bottom, make to mark at the center of dropwise addition after air-drying, is i.e. expansion is former
Point;Substrate oblique cutting is entered in cuvette, it is about 70 ° to have the face-up of sample, angle, covers glass slide, makes methanol in substrate
Freely it is unfolded with pigment point;After methanol can not continue expansion, it is to be detected to take out substrate natural air drying.
3, substrate is placed under Raman spectrometer probe, surface sweeping initial point is that sample origin is added dropwise, every along expansion direction
5 random points are scanned every 1mm, the characteristic peak in spectrum is analyzed.The results show that red (AR) is lured to be different from other pigments
Characteristic peak be located at 752cm-1And 1272cm-1;The characteristic peak that amaranth (AM) is different from other pigments is located at 1345cm-1With
1361cm-1;The characteristic peak that sunset yellow (SY) is different from other pigments is located at 986cm-1And 1332cm-1;Brilliant blue (BB) is different from it
The characteristic peak of his pigment is located at 917cm-1And 1618cm-1;The characteristic peak that lemon yellow (TA) is different from other pigments is located at 1128cm-1And 1595cm-1;The characteristic peak that indigo (IN) is different from other pigments is located at 674cm-1And 575cm-1.6 kinds of pigments respectively pass through
After UTLC expansion, is detected by SERS, obtain the relationship of its feature peak intensity and development distance.It can be obtained after normalization various
Situation is unfolded in the UTLC of pigment, has advanced in total L=14mm in conjunction with solvent front, has obtained luring red development distance being 5mm<
LAR<10mm, Rf value 0.36<RfAR<0.71, characteristic peak most strong position is located at 8mm, corresponding RfARmax=0.57;Indigo
Development distance is 3mm<LIN<9mm, Rf value 0.21<RfIN<0.64, characteristic peak most strong position is located at 8mm, corresponding RfINmax
=0.57;The development distance of lemon yellow is 2mm<LTA<8mm, Rf value 0.36<RfTA<0.71, characteristic peak most strong position is located at
At 4mm, corresponding RfTAmax=0.29;The development distance of brilliant blue is 0mm<LBB<5mm, Rf value 0<RfBB<0.36, characteristic peak is most
Strong position is located at 1mm, corresponding RfBBmax=0.07;The development distance of sunset yellow is 3mm<LSY<8mm, Rf value 0.21<RfSY
<0.57, characteristic peak most strong position is located at 5mm, corresponding RfSYmax=0.36;The development distance of amaranth is 5mm<LAM<7mm, than
Shifting value is 0.36<RfAM<0.5, characteristic peak most strong position is located at 6mm, corresponding RfAMmax=0.43.
This method shows that Silver nanorod array substrate can be used as Development of Thin-Layer Chromatography to be detected with Surface enhanced Raman spectroscopy
Substrate, and this method can fast and accurately detect 6 kinds of synthetic food colors.
Claims (6)
1. a kind of method of TLC technique and Surface enhanced Raman spectroscopy technology combination detection synthetic food color, feature
It is:Include the following steps:
A, the preparation of Silver nanorod array substrate:Titanium film is deposited in glass substrate surface and silver is thin using glancing angle deposition technology
Film continues deposition of silver nanometer rods after adjusting deposition angles;
B, Development of Thin-Layer Chromatography:Thin-layer chromatography exhibition is carried out to the synthetic food color in Silver nanorod array substrate using methanol
It opens;
C, Surface enhanced Raman spectroscopy detects:Raman spectrum detection is carried out to the sample after expansion.
2. a kind of TLC technique according to claim 1 and the artificial conjunction of Surface enhanced Raman spectroscopy technology combination detection
At the method for pigment, it is characterised in that:The preparation method of the Silver nanorod array substrate is as follows:By long 2.5cm, wide 0.5cm
Glass substrate be fixed on sample stage surface and be right against steam incident direction, when film deposition vacuum cavity air pressure be less than 10- 6When Torr, the titanium film of one layer of 20nm is deposited in glass substrate surface using electron beam deposition coating method, waits for film deposition vacuum
Cavity continues that the Ag films of one layer of 100nm are deposited to form bottom surface enhancing Raman scattering knot after being cooled to the solidification of titanium film material
Structure makes sample stage normal with steam incident direction in 85 ° after cavity is cooled to the solidification of silverskin material, continues that 2000nm silver is deposited
Film enhances Raman scattering Silver nanorod array structure to form upper surface.
3. a kind of TLC technique according to claim 2 and the artificial conjunction of Surface enhanced Raman spectroscopy technology combination detection
At the method for pigment, it is characterised in that:The Development of Thin-Layer Chromatography method is as follows:In a long 2cm, wide 2cm, the stone of high 3cm
600 μ L absolute methanols are added in English cuvette;It is placed on cuvette mouth using a piece of clean glass slide, 1min is waited for make cuvette
In absolute methanol atmosphere saturation;On Silver nanorod array substrate surface from 2 μ L people of dropwise addition at the bottom 0.5cm of nanowire growth direction
Work synthetic dyestuff sample, at the center of dropwise addition origin is unfolded to mark in work after air-drying;Silver nanorod array substrate oblique cutting is entered
In quartz colorimetric utensil, it is 70 °~75 ° to have the face-up of sample, angle, covers glass slide, makes methanol in Silver nanorod array base
Freely it is unfolded with pigment point on bottom;After absolute methanol can not continue expansion, Silver nanorod array substrate natural air drying is taken out
It is to be detected.
4. a kind of TLC technique according to claim 3 and the artificial conjunction of Surface enhanced Raman spectroscopy technology combination detection
At the method for pigment, it is characterised in that:The Raman spectrum method for detecting surface reinforcement is as follows:Substrate is placed in Raman spectrometer
Under probe, surface sweeping initial point is that sample origin is added dropwise, and 5 random points is scanned every 1mm along expansion direction, to the spy in spectrum
It is analyzed at sign peak.
5. a kind of TLC technique according to claim 2 and the artificial conjunction of Surface enhanced Raman spectroscopy technology combination detection
At the method for pigment, it is characterised in that:Glass substrate is fixed on by sample stage surface using Teflon adhesive tape.
6. being examined according to a kind of TLC technique of claim 1-5 any one of them and the combination of Surface enhanced Raman spectroscopy technology
The method for surveying synthetic food color, it is characterised in that:The sample stage is using round stainless steel sample stage.
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Citations (7)
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| US8810789B2 (en) * | 2011-11-07 | 2014-08-19 | University Of Georgia Research Foundation, Inc. | Thin layer chromatography-surfaced enhanced Raman spectroscopy chips and methods of use |
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2018
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Patent Citations (7)
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| US8810789B2 (en) * | 2011-11-07 | 2014-08-19 | University Of Georgia Research Foundation, Inc. | Thin layer chromatography-surfaced enhanced Raman spectroscopy chips and methods of use |
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