CN113834777B - Preparation and application methods of SERS substrate for detecting acidic pigment - Google Patents
Preparation and application methods of SERS substrate for detecting acidic pigment Download PDFInfo
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- CN113834777B CN113834777B CN202110800116.3A CN202110800116A CN113834777B CN 113834777 B CN113834777 B CN 113834777B CN 202110800116 A CN202110800116 A CN 202110800116A CN 113834777 B CN113834777 B CN 113834777B
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- 239000000758 substrate Substances 0.000 title claims abstract description 64
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 title claims abstract description 40
- 239000000049 pigment Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 21
- 230000002378 acidificating effect Effects 0.000 title claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- 238000002791 soaking Methods 0.000 claims description 33
- 239000002253 acid Substances 0.000 claims description 20
- GFLJTEHFZZNCTR-UHFFFAOYSA-N 3-prop-2-enoyloxypropyl prop-2-enoate Chemical compound C=CC(=O)OCCCOC(=O)C=C GFLJTEHFZZNCTR-UHFFFAOYSA-N 0.000 claims description 15
- 229920000371 poly(diallyldimethylammonium chloride) polymer Polymers 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 10
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 claims description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 238000011010 flushing procedure Methods 0.000 claims description 8
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 7
- 239000008103 glucose Substances 0.000 claims description 7
- 238000012360 testing method Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000011065 in-situ storage Methods 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 13
- 238000005520 cutting process Methods 0.000 abstract description 3
- 238000010521 absorption reaction Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 28
- 235000009328 Amaranthus caudatus Nutrition 0.000 description 12
- 240000001592 Amaranthus caudatus Species 0.000 description 12
- 239000004178 amaranth Substances 0.000 description 12
- 235000012735 amaranth Nutrition 0.000 description 12
- SGHZXLIDFTYFHQ-UHFFFAOYSA-L Brilliant Blue Chemical group [Na+].[Na+].C=1C=C(C(=C2C=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C=2C(=CC=CC=2)S([O-])(=O)=O)C=CC=1N(CC)CC1=CC=CC(S([O-])(=O)=O)=C1 SGHZXLIDFTYFHQ-UHFFFAOYSA-L 0.000 description 7
- 238000001069 Raman spectroscopy Methods 0.000 description 7
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000000835 fiber Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000000523 sample Substances 0.000 description 5
- 238000000479 surface-enhanced Raman spectrum Methods 0.000 description 5
- 239000003638 chemical reducing agent Substances 0.000 description 4
- 230000035945 sensitivity Effects 0.000 description 4
- 239000000975 dye Substances 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 239000001040 synthetic pigment Substances 0.000 description 3
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 2
- 238000007605 air drying Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000005251 capillar electrophoresis Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000840 electrochemical analysis Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000004557 single molecule detection Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 1
Classifications
-
- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
-
- 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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- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)
Abstract
The application discloses a preparation method and a use method of an SERS substrate for detecting acidic pigment, wherein the preparation method of the SERS substrate for detecting the acidic pigment comprises the following steps: the base for detection prepared by the application has the advantages of simple manufacture, low cost, convenient carrying, good water absorption and convenient cutting.
Description
Technical Field
The application relates to the technical field of test paper manufacturing, in particular to a preparation method and a use method of an SERS substrate for detecting acidic pigment.
Background
At present, conventional methods for identifying artificially synthesized pigments comprise a capillary electrophoresis method (Capillary Electrophoresis, CE), an electrochemical analysis method (Electrochemical Analysis), a high performance liquid chromatography method (High Performance Liquid Chromatography, HPLC) and the like, however, the conventional methods have the defects of complex sample pretreatment, complicated operation, long time consumption, high detection cost and the like, and are only suitable for laboratory detection, and cannot meet the requirements of on-site rapid screening. Accordingly, there is an increasing effort to develop new methods for rapid, simple detection of artificial dyes in food products.
Surface Enhanced Raman (SERS) analysis techniques are molecular structure characterization methods established based on raman effects and nanotechnology. Surface plasmon resonance generated by noble metal nanomaterial such as gold and silver can amplify molecular Raman signal adsorbed on surface of SERS substrate by about 10 6 ~10 14 Multiple times, some can even realize single molecule detection. Compared with other analysis methods, the SERS technology has the advantages of no need of a special complex sample pretreatment process, high sensitivity, strong specificity, no interference by water, capability of realizing on-site rapid detection by combining with a portable Raman instrument, and the like, and has strong application potential in the field of pigment detection.
In recent years, researchers have been trying and developing new methods for rapid detection of synthetic pigments in foods using surface enhanced raman. However, a great deal of research shows that acidic dye molecules with negative charges, such as amaranth, sunset yellow, allure red and the like, have weak affinity to gold or silver, are not easy to adsorb and enrich on the surface of a substrate, and are difficult to directly detect by SERS. Therefore, the SERS substrate for detecting the acid artificial synthetic pigment with high sensitivity is constructed, and the research on the SERS detection method of the acid artificial synthetic pigment is very important.
Disclosure of Invention
This section is intended to outline some aspects of embodiments of the application and to briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section as well as in the description of the application and in the title of the application, which may not be used to limit the scope of the application.
The present application has been made in view of the above and/or problems occurring in the prior art for detecting acidic pigment products.
Therefore, one of the purposes of the application is to overcome the defects of the detection of acid pigment products and provide a preparation method of a SERS substrate for detecting acid pigment.
In order to solve the above technical problems, according to one aspect of the present application, the following technical scheme is provided: a method for preparing a SERS substrate for detecting an acidic dye, comprising the steps of:
manufacturing a filter paper substrate: preparing silver ammonia solution, soaking filter paper in the silver ammonia solution, and reducing the silver ammonia solution adsorbed on the surface of the filter paper in situ by using a reducing agent to prepare a filter paper substrate;
flushing and soaking: washing the prepared filter paper substrate by using the solution, and then immersing the filter paper substrate in PDDA solution for immersing;
airing and soaking again: and (3) drying the filter paper substrate subjected to washing and soaking treatment, then washing with the solution and water, then putting into a PDDA solution for soaking again, airing, putting into the PDDA solution for soaking, and airing again for later use.
As a preferable scheme of the preparation method of the SERS substrate for detecting the acid pigment, the preparation method comprises the following steps: in the manufacture of the filter paper substrate, the reducing agent is glucose.
As a preferable scheme of the preparation method of the SERS substrate for detecting the acid pigment, the preparation method comprises the following steps: and in the steps of flushing, soaking, airing and re-soaking, the solution is one or more of organic solution, inorganic solution and water.
As a preferable scheme of the preparation method of the SERS substrate for detecting the acid pigment, the preparation method comprises the following steps: in the washing and soaking, the used solution comprises glucose solution, ethanol solution and deionized water.
As a preferable scheme of the preparation method of the SERS substrate for detecting the acid pigment, the preparation method comprises the following steps: in the air drying and re-soaking, the used solution includes water and ethanol solution.
As a preferable scheme of the preparation method of the SERS substrate for detecting the acid pigment, the preparation method comprises the following steps: in the air drying and re-soaking, the washing times of the ethanol solution and the water are 3 times.
As a preferable scheme of the preparation method of the SERS substrate for detecting the acid pigment, the preparation method comprises the following steps: in the rinsing, soaking, airing and re-soaking, the concentration of the PDDA solution was 0.1%.
As a preferable scheme of the preparation method of the SERS substrate for detecting the acid pigment, the preparation method comprises the following steps: and in the steps of airing and re-soaking, airing at normal temperature.
As a preferable scheme of the preparation method of the SERS substrate for detecting the acid pigment, the preparation method comprises the following steps: the time of soaking in PDDA solution in the washing, soaking, airing and re-soaking is 30min.
As a preferable scheme of the preparation method of the SERS substrate for detecting the acid pigment, the preparation method comprises the following steps: the pigment was selected and measured using a raman spectrometer.
The application discloses a preparation method and a detection method of an SERS substrate for detecting acid pigments, which have the advantages of high sensitivity, strong specificity, no interference by water, simple preparation, low cost, portability, good water absorbability, biodegradability, easiness in cutting into different shapes and sizes and the like on the basis of realizing the effect of rapid detection.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art. Wherein:
FIG. 1 is an SEM image of the lower Ag NPs-filter paper substrate prepared in example 1 at various magnifications;
FIG. 2 is a SERS spectrum of the Ag NPs-filter paper substrate prepared in example 2 with and without PDDA modification;
in the figure, a is amaranth, b is brilliant blue, c is sunset yellow, and d is allure red;
FIG. 3 is a SERS spectrum of prepared filter paper and acid pigments of different concentrations;
in the figure, a is amaranth, and b is brilliant blue;
FIG. 4 is a SERS plot of 5ppm amaranth measured on an Ag NPs-filter paper substrate
In the figure, a is different test points, and b is different substrates.
Detailed Description
In order that the above-recited objects, features and advantages of the present application will become more apparent, a more particular description of the application will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present application, but the present application may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present application is not limited to the specific embodiments disclosed below.
Further, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic can be included in at least one implementation of the application. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
Dropwise adding 2% ammonia water solution into 20mL of 5mM AgNO at normal temperature and normal pressure 3 In the solution, until the precipitate in the mixed solution completely disappeared, the volume was fixed in a 25mL volumetric flask to prepare a 4mM silver-ammonia solution. Then, the prepared filter paper is put into a culture dish (the filter paper is firstly cleaned by deionized water), 10mL of 4mM silver-ammonia solution is poured into the culture dish, the culture dish is shaken to soak the filter paper and the filter paper is kept stand for a period of time, so that Ag (NH) in the solution 3 ) 2 + Fully adsorbing on the surface of filter paper, then dripping 0.3mL of 12% glucose solution, shaking uniformly, and standing for 18h. Under the action of reducing agent, silver mirror reaction starts to occur, ag (NH) 3 ) 2 + The silver nano particles are slowly reduced by the reducing agent, and the culture dish is not required to be moved in the reaction process so as not to damage the reaction system, so that the silver nano particles are unevenly or infirm attached. After the reaction is carried out for a period of time, the solution turns from transparent to green and finally turns to dark green, and the reaction is finished. And after the reaction is finished, taking out the filter paper, sequentially flushing with water and ethanol for 3 times, removing reactants adsorbed on the surface, and naturally airing at room temperature for later use. Soaking the prepared Ag-filter paper substrate in 0.1% PDDA solution for 30min, taking out, and naturally airing at room temperature for later use. SEM pictures of the prepared filter paper substrate at different magnifications are shown in fig. 1.
Example 2
The enhancement effect of the filter paper substrate on the acid pigment is compared with that of the filter paper substrate modified by using the Ag NPs-filter paper substrate and the PDDA, and the enhancement effect of the filter paper substrate on the acid pigment is detected in the following manner: the SERS spectra of 20ppm of allure red, amaranth, brilliant blue, sunset yellow on PDDA modified and unmodified Ag NPs-filter paper substrates were tested with the probe molecules. The resulting spectrum is shown in FIG. 2.
Example 3
And (3) selecting acid pigment amaranth, alluring red, brilliant blue and sunset yellow as solutions to be detected, wherein in SERS measurement, all SERS spectrums are obtained by adopting a DXR micro-Raman spectrometer, a 780nm laser is assembled, and the laser power is 5mW and the exposure time is 10s. The laser beam is microscopically positioned through a 10X eyepiece, and the laser spot is 3 μm. Cutting an Ag NPs-filter paper substrate into small paper sheets with the thickness of 2X 4mm, soaking the small paper sheets into 1mL of to-be-tested liquid with different concentrations for 20min, taking out the small paper sheets, placing the small paper sheets on a clean glass slide, and carrying out SERS test after the solution volatilizes, wherein each sample is tested for 3 times. The resulting SERS image is shown in fig. 3.
Example 4
The amaranth is used as probe molecule to test the precision of different test points and different substrates on the same substrate, and the test is set as follows, 1338cm amaranth -1 Peak intensity calculation RSD was 6.8%, 5 batches of substrates were prepared under the same conditions, 5 spots were randomly tested on each substrate, and the resulting image is shown in fig. 4.
As can be seen from fig. 1, the filter paper is composed of a plurality of interweaved fibers, the fibers are composed of smaller fibers, a multi-layer three-dimensional structure substrate is provided for nano silver, and a plurality of nano silver particles are densely distributed on each fiber. As the magnification is further increased, as can be seen in the maximum resolution image of fig. 1, ag NPs particles on the surface of the filter paper substrate appear nearly spherical, with uniform particle size, and particles stacked close to each other, forming a large number of "hot spots", which are beneficial for producing strong SERS effects.
As can be seen from FIG. 2, 20ppm of SERS of brilliant blue and sunset yellow could be detected on an Ag NPs-filter paper substrate without modification of PDDA, and no significant SERS signal was detected for both amaranth and allure. This is because the acidic molecules such as amaranth and allure have weak forces with the Ag NPs-filter paper substrate and are not easily adsorbed to the substrate surface, so that the SERS signal is difficult to detect. On the Ag NPs-filter paper substrate, the peaks of the four pigments are obviously enhanced. Because a large number of hot spots are formed among the high-density nano silver particles on the surface of the Ag NPs-filter paper substrate, electronegative pigment molecules can be enriched into SERS 'hot spot' areas through the electrostatic action of PDDA and the capillary action of filter paper fibers, so that the SERS sensitivity of the Ag NPs-filter paper substrate is greatly improved.
As can be seen from fig. 3, the SERS spectrum signal of both amaranth and brilliant blue decreases with decreasing concentration. The minimum detection concentrations of amaranth and brilliant blue for the PDDA-modified Ag NPs filter paper substrate were 1ppm and 0.01ppm, respectively.
The substrate for detecting the acid pigment is prepared in the application, and the preparation method has the advantages of simple process, low cost and good reproducibility of detection effect.
It should be noted that the above embodiments are only for illustrating the technical solution of the present application and not for limiting the same, and although the present application has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present application may be modified or substituted without departing from the spirit and scope of the technical solution of the present application, which is intended to be covered in the scope of the claims of the present application.
Claims (8)
1. A preparation method of an SERS substrate for detecting acidic pigment is characterized by comprising the following steps of: the method comprises the following steps:
manufacturing a filter paper substrate: preparing silver ammonia solution, soaking filter paper in the silver ammonia solution, and reducing the silver ammonia solution adsorbed on the surface of the filter paper in situ by using glucose solution to prepare a filter paper substrate, wherein the concentration of the silver ammonia solution is 4mM, the concentration of the glucose solution is 12%, and the ratio of the glucose solution to the silver ammonia solution is 0.3mL:10mL;
flushing and soaking: washing the prepared filter paper substrate by using the solution, and then immersing the filter paper substrate in PDDA solution for 30min;
airing and soaking again: and (3) drying the filter paper substrate subjected to washing and soaking treatment, then washing with the solution and water, then putting into a PDDA solution for soaking again, airing, putting into the PDDA solution for soaking, and airing again for later use.
2. The method for preparing the acid pigment test paper according to claim 1, wherein: in the steps of flushing, soaking, airing and re-soaking, the solution is one or more of organic solution, inorganic solution and water.
3. The method for preparing the SERS substrate for detecting acidic pigments according to claim 1, wherein: in the flushing and soaking, the used solution comprises glucose solution, ethanol solution and deionized water.
4. The method for preparing the SERS substrate for detecting acidic pigments according to claim 1, wherein: in the airing and re-soaking, the used solution comprises water and ethanol solution.
5. The method for preparing a SERS substrate for detecting acidic pigments according to claim 4, wherein: in the steps of airing and re-soaking, the flushing times of the ethanol solution and the water are 3 times.
6. The method for preparing a SERS substrate for detecting acidic pigments according to claim 1, wherein: in the flushing, soaking, airing and re-soaking, the concentration of the PDDA solution is 0.1%.
7. The method for preparing a SERS substrate for detecting acidic pigments according to claim 1, wherein: and in the steps of airing and re-soaking, airing is carried out at normal temperature.
8. Use of a SERS substrate prepared by the method of any one of claims 1 to 7 for detecting acidic pigments.
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CN105223183A (en) * | 2015-09-18 | 2016-01-06 | 中国科学院生态环境研究中心 | A kind of substrate that can be used for zwitterion pigment selective enumeration method |
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