CN112051255A - Application of nano copper-based semiconductor compound in Sudan red specificity detection - Google Patents
Application of nano copper-based semiconductor compound in Sudan red specificity detection Download PDFInfo
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Images
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
- G01N21/62—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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses an application of a nano copper-based semiconductor compound in Sudan red specificity detection. The invention also provides a method for detecting the specificity of Sudan red, which comprises the following steps: the method comprises the following steps of (1) taking a nano copper-based semiconductor compound as an SERS active substrate material; or providing the aforementioned SERS-active substrate material; and contacting the SERS active substrate material with a detection sample possibly containing Sudan red, and detecting by using a Raman spectrometer to realize the specific detection of the Sudan red. Compared with the existing commercialized precious metal substrate material, the nano copper-based semiconductor compound is used as the SERS active substrate material, so that the method has the advantages of low cost, high selectivity and the like, and the specificity and semi-quantitative detection of the Sudan red additive in food can be realized by the technology; the SERS active substrate material is simple to prepare, low in cost, suitable for large-scale mass production and capable of directly and rapidly detecting target molecules in a semi-quantitative mode.
Description
Technical Field
The invention belongs to the technical field of spectroscopy and molecular recognition, and particularly relates to application of a copper-based nano semiconductor compound in Sudan red specificity detection, in particular to a method for performing specificity and semi-quantitative detection on illegally added Sudan red molecules in food by using a copper-based nano semiconductor compound substrate based on an SERS (surface enhanced Raman scattering spectroscopy) technology.
Background
Sudan red is a kind of azo compound using phenyl azo naphthol as main group, mainly including Sudan red I, II, III and IV. The chemical names are 1-phenylazo-2-naphthol, 1- [ (2, 4-dimethylbenzene) azo ] -2-naphthol, 1- [4- (phenylazo) phenyl ] azo-2-naphthol, and 1-2-methyl-4- [ (2-methylbenzene) azo ] phenylazo-2-naphthol, respectively. The compound is insoluble in water, slightly soluble in ethanol, and easily soluble in acetone, benzene, diethyl ether, n-hexane, oil, etc. Sudan red belongs to artificially synthesized red dye and is mainly used for the hyperchromic and brightening of solvents, oil, wax, floors, shoes and the like. Sudan red has been banned as a food pigment in countries such as the European Union as early as 1995, but since 2005, Sudan red has been detected in a large number of products such as chili sauce, chili powder, new Orleans roasted wings, duck eggs and the like, which are well-known and across-country companies and domestic enterprises. The addition of the Sudan red in the food causes great harm to the health of human bodies, and in a plurality of in vitro experiments, the Sudan red is found to enter the human bodies and can be metabolized to generate aniline substances and naphthylamine substances, and the amine substances have mutagenicity and carcinogenicity. The International agency for research on cancer (IARC) will be listed as three carcinogens of Sudan red I, II, III and IV, namely animal carcinogens. In 4.2005, the Ministry of health issued the Sudan Red Risk assessment report, which states that if food containing higher dose of Sudan Red is taken frequently, the risk of carcinogenesis is increased, especially because the metabolite of Sudan Red is carcinogen possible for human, and there is no data on the tolerance of intake of these substances, so that the intake of these substances should be avoided as much as possible.
The first and fifth batches of the national publication list of varieties of non-edible substances and easily abusable food additives which are possibly illegally added into foods have listed Sudan red as a non-edible substance which is prohibited to be added. Aiming at the problem that Sudan red which is a natural substance in non-food is frequently detected in food, the detection of Sudan red is always the key point of supervision and spot check and risk monitoring work of functional departments. In 2019, the national food safety selective inspection implementation rules stipulate that food such as spice oil, hot pepper and products thereof, pickled vegetables containing hot pepper and dried vegetable products, egg products, cakes added with eggs in raw materials and the like must be detected for Sudan red.
The method for detecting Sudan red mainly comprises enzyme-linked immunosorbent assay, surface enhanced Raman spectroscopy, infrared spectroscopy, thin-layer chromatography, liquid chromatography-mass spectrometry and the like. The GB/T19681-2005 [10] pretreatment adopts a self-filled neutral alumina chromatographic column, the activity of alumina is required to be adjusted according to the recovery rate of Sudan red before use, the requirement on the experience of detection personnel is high, the parallelism and the accuracy are poor, and a large amount of organic solvent is consumed.
The Surface Enhanced Raman Spectroscopy (SERS) is a high-selectivity and ultrasensitive rapid surface analysis technology, and lays a theoretical foundation for realizing rapid specificity and semi-quantitative detection of Sudan red in food. However, most of the existing commercial SERS substrates are based on the nano-structures of gold, silver and other precious metal materials, the currently disclosed method for detecting sudan red in food based on SERS usually uses gold sol as a substrate, and due to the indiscriminate amplification of raman signals of substrate components by the electromagnetic enhancement effect of the precious metal substrate, the detection mostly needs a complex pretreatment process, and the problems of long time consumption, high cost, poor selectivity, poor stability and the like are faced, so that the practical application is limited. Therefore, the method for detecting the Sudan red in the food, which is rapid and efficient, simple to operate, low in cost and capable of effectively identifying the Sudan red, has great significance.
Disclosure of Invention
The invention mainly aims to provide an application of a nano copper-based semiconductor compound in the specific detection of Sudan red so as to overcome the defects of the prior art.
The invention also aims to provide a method for specifically detecting Sudan red by using the nano copper-based semiconductor compound as a SERS active substrate material.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides application of a copper-based semiconductor compound serving as a SERS active substrate material in Sudan red specificity detection, wherein the copper-based semiconductor compound comprises Cu with a hollow structure2O-base material and/or MOF-Cu of core-shell structure2And (3) O base material.
The embodiment of the invention also provides a SERS active substrate material for Sudan red specificity detection, which comprises a nano copper-based semiconductor compound, wherein the nano copper-based semiconductor compound comprises Cu with a hollow structure2O-base material and/or MOF-Cu of core-shell structure2And (3) O base material.
The embodiment of the invention also provides a preparation method of the SERS active substrate material for danhong specificity detection, which comprises the following steps:
reacting a first mixed reaction system containing copper chloride, sodium hydroxide, a reducing agent and water at room temperature for 30min to prepare Cu with a hollow structure2An O base material;
or reacting a second mixed reaction system containing copper chloride, sodium hydroxide, a reducing agent and water at room temperature for 15min to obtain Cu with a solid structure2O; thereafter, the Cu containing the solid structure2Carrying out hydrothermal reaction on a third mixed reaction system of O, terephthalic acid, 4-4' bipyridine, ethanol and water at 90 ℃ for 6h to prepare the MOF-Cu with the core-shell structure2And (3) O base material. The embodiment of the invention also provides a Sudan red specificity detection method, which comprises the following steps:
the method comprises the following steps of (1) taking a nano copper-based semiconductor compound as an SERS active substrate material; or providing the aforementioned SERS-active substrate material;
and contacting the SERS active substrate material with a detection sample possibly containing Sudan red, and detecting by using a Raman spectrometer to realize the specific detection of the Sudan red.
Compared with the prior art, the invention has the beneficial effects that:
(1) the copper-based semiconductor compound prepared by the invention is prepared by designing a novel cuprous oxide hollow structure and MOF-Cu2O core-shell structure, changing surface chemical structure of substrate to realize substrateThe sensitivity and the specific adsorption effect on the sudan red molecules enable the sudan red molecules to be selectively adsorbed from common typical complex food systems such as chili sauce, chili oil, tomato sauce, mayonnaise, sausage and the like, the quick detection and identification of the sudan red dye can be realized without complex pretreatment, and a very valuable reference is provided for developing a low-cost SERS detection technology;
(2) the SERS active substrate material for detecting the specificity of Sudan red is simple to prepare, low in cost, simple to operate, quick and effective; most importantly, the method can realize the specificity and semi-quantitative detection of the sudan red molecule and can effectively identify and appraise the sudan red molecule.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 Cu of the present invention in the form of a hollow nanocube structure in example 12The enhanced Raman spectrogram of O as SERS active substrate for different series of Sudan red probe molecules;
FIG. 2 is a MOF-Cu core-shell structure in example 2 of the present invention2Enhanced raman spectra of O as SERS active substrate for different concentrations of sudan red probe molecules (sudan red No. 3);
FIG. 3 shows Cu of hollow nanocube structure in examples 3 to 6 of the present invention2The enhanced Raman spectrogram of O serving as an SERS active substrate for chilli powder, tomato sauce, chilli oil and sausage;
FIG. 4 shows Cu of the hollow nanocube structure of example 72The enhanced Raman spectrogram of the O substrate and the Ag sol on the mixed pigment molecules respectively,
FIGS. 5a to 5c are Cu of solid cubic structure in comparative example 1 of the present invention2O, Cu of nano hollow cubic structure prepared in example 12O, core-Shell MOF-Cu prepared in example 22An electron micrograph of O;
FIG. 6 shows Cu of nano hollow cubic structure prepared in example 1 of the present invention2O substrate and Cu of solid cubic structure prepared in comparative example 12Concentration of O pair is 10-4Enhanced Raman spectra of mol/L Sudan Red.
Detailed Description
In view of the defects of the prior art, the inventor of the present invention has long studied and largely practiced to propose the technical solution of the present invention, which will be clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The Surface Enhanced Raman Spectroscopy (SERS) is a high-selectivity and ultrasensitive rapid surface analysis technology, and lays a theoretical foundation for realizing rapid specificity and semi-quantitative detection of Sudan red in food. In recent years, a semiconductor compound has been studied as a SERS active substrate. The semiconductor compound material is used as an SERS active substrate, so that on one hand, the enhancement factor can be effectively improved, and the detection limit of target molecules is reduced; on the other hand, the probe also has good stability and probe molecule selectivity.
One aspect of the embodiment of the invention provides an application of a nano copper-based semiconductor compound as a SERS active substrate material in Sudan red specificity detection, wherein the nano copper-based semiconductor compound comprises Cu with a hollow structure2O-base material and/or MOF-Cu of core-shell structure2And (3) O base material.
The new SERS technology for performing specificity detection on Sudan red by using the nano copper-based semiconductor compound as an SERS active substrate material comprises the steps of preparing the SERS active substrate material (the nano copper-based semiconductor compound) by a chemical method, directly mixing the substrate material with the Sudan red, and performing direct and rapid detection under a Raman optical spectrometer after adsorption balance is achieved.
In some more specific embodiments, the method for preparing the nano copper-based semiconductor compound comprises the following steps:
reacting a first mixed reaction system containing copper chloride, sodium hydroxide, a reducing agent and water at room temperature for 30min to prepare Cu with a hollow structure2An O base material;
or reacting a second mixed reaction system containing copper chloride, sodium hydroxide, a reducing agent and water at room temperature for 15min to obtain Cu with a solid structure2O; thereafter, the Cu containing the solid structure2Carrying out hydrothermal reaction on a third mixed reaction system of O, terephthalic acid, 4-4' bipyridine, ethanol and water at 90 ℃ for 6h to prepare the MOF-Cu with the core-shell structure2And (3) O base material.
In some more specific embodiments, the reducing agent comprises L-ascorbic acid or glucose, preferably L-ascorbic acid.
Further, MOF-Cu of the core-shell structure2The core of the O substrate material is cuprous oxide, and the shell is MOF structure.
Further, MOF-Cu of the core-shell structure2The particle size of the core in the O-based material is 245-255nm, and preferably 250 nm.
Further, MOF-Cu of the core-shell structure2The thickness of the shell in the O-base material is 100-200nm, preferably 150 nm.
Further, the molar concentration ratio of the copper chloride, the sodium hydroxide and the reducing agent in the first mixed reaction system is 1:1: 1.
Further, the molar concentration ratio of the copper chloride, the sodium hydroxide and the reducing agent in the second mixed reaction system is 1:20: 1.
Further, Cu of a solid structure in the third mixed reaction system2The molar concentration ratio of O, terephthalic acid and 4-4' bipyridyl is 3:2: 4.
Further, the sudan red includes any one or a combination of two or more of sudan red No. 1, sudan red No. 3, sudan red B and sudan red G, and is not limited thereto.
In another aspect of the embodiments of the present invention, there is also provided a SERS active substrate material for sudan red specificity detection, comprising a nano copper-based semiconductor compound including Cu having a hollow structure2O-base material and/or MOF-Cu of core-shell structure2And (3) O base material.
In another aspect of the embodiments of the present invention, there is provided a method for preparing the SERS-active substrate material for sudan red specificity detection, including:
reacting a first mixed reaction system containing copper chloride, sodium hydroxide, a reducing agent and water at room temperature for 30min to prepare Cu with a hollow structure2An O base material;
or reacting a second mixed reaction system containing copper chloride, sodium hydroxide, a reducing agent and water at room temperature for 15min to obtain Cu with a solid structure2O; thereafter, the Cu containing the solid structure2Carrying out hydrothermal reaction on a third mixed reaction system of O, terephthalic acid, 4-4' bipyridine, ethanol and water at 90 ℃ for 6h to prepare the MOF-Cu with the core-shell structure2And (3) O base material.
In the invention, cupric salt containing divalent ions can also replace cupric chloride to prepare the SERS active substrate material for detecting the specificity of Sudan red.
In some more specific embodiments, the reducing agent comprises L-ascorbic acid or glucose, preferably L-ascorbic acid.
Further, MOF-Cu of the core-shell structure2The core of the O substrate material is cuprous oxide, and the shell is MOF structure.
Further, MOF-Cu of the core-shell structure2The particle size of the core in the O-based material is 245-255nm, and preferably 250 nm.
Further, MOF-Cu of the core-shell structure2The thickness of the shell in the O-base material is 100-200nm, preferably 150 nm.
Further, the molar concentration ratio of the copper chloride, the sodium hydroxide and the reducing agent in the first mixed reaction system is 1:1: 1.
Further, the molar concentration ratio of the copper chloride, the sodium hydroxide and the reducing agent in the second mixed reaction system is 1:20: 1.
Further, Cu of a solid structure in the third mixed reaction system2The molar ratio of O, terephthalic acid and 4-4' bipyridyl is 3:2: 4.
In another aspect of the embodiments of the present invention, a method for detecting sudan red specificity is provided, which includes:
the method comprises the following steps of (1) taking a nano copper-based semiconductor compound as an SERS active substrate material; or providing the aforementioned SERS-active substrate material;
and contacting the SERS active substrate material with a detection sample possibly containing Sudan red, and detecting by using a Raman spectrometer to realize the specific detection of the Sudan red.
Further, the sudan red includes any one or a combination of two or more of sudan red No. 1, sudan red No. 3, sudan red B and sudan red G, and is not limited thereto.
In some embodiments, the sudan red specific detection method comprises:
directly mixing the solution dispersed with certain content of copper-based semiconductor compound substrate material with food extract of Sudan red to reach adsorption balance. Then, after a certain amount of mixed solution is dripped on a clean silicon wafer to be dried, the Sudan red can be directly detected by using a Raman spectrometer, and the Raman-enhanced food additive has an obvious Raman enhancement effect on the Sudan red, and can efficiently identify and semi-quantitatively detect the Sudan red molecules contained in food.
Further, dispersing the prepared nano copper-based semiconductor compound substrate material into a certain amount of ethanol to obtain an ethanol solution of the nano copper-based semiconductor compound substrate material, then taking a certain amount of the solution, adding Sudan red ethanol solutions with different concentrations, standing in a dark place, dropping a certain amount of mixed solution into clean Si/SiO2And (4) naturally drying the substrate, testing the substrate on a Raman spectrometer, and collecting data.
Further, the test sample includes sudan red, or a mixture of sudan red and chilli sauce, etc.
The copper-based semiconductor compound prepared by the invention is prepared by designing a novel cuprous oxide hollow structure and MOF-Cu2The O core-shell structure changes the surface chemical structure of the substrate, realizes the sensitivity and specific adsorption of the substrate to Sudan red molecules, enables the substrate to selectively adsorb the Sudan red molecules from common typical complex food systems such as chili sauce, chili oil, tomato sauce, mayonnaise, sausage and the like, and realizes the rapid detection and identification of the Sudan red dye without complex pretreatment.
The copper-based semiconductor compound material with the modified surface is mainly used as an SERS active substrate material, so that direct, rapid and specific and semi-quantitative detection of Sudan red molecules contained in foods such as chilli powder, chilli oil, tomato sauce, mayonnaise and sausage and mixed pigments is realized, various Sudan red dye molecules can be involved, certain universality is achieved, the Raman signal of the Sudan red can be greatly and selectively enhanced in Raman detection, and the addition of the Sudan red in the foods can be effectively identified and identified.
The technical solutions of the present invention are further described in detail below with reference to several preferred embodiments and the accompanying drawings, which are implemented on the premise of the technical solutions of the present invention, and a detailed implementation manner and a specific operation process are provided, but the scope of the present invention is not limited to the following embodiments.
The experimental materials used in the examples used below were all available from conventional biochemical reagents companies, unless otherwise specified.
Example 1
Under magnetic stirring, adding CuCl2(1mL, 0.1mol/L), NaOH solution (1mL, 0.1mol/L) and distilled water (40mL) are mixed, L-ascorbic acid (1mL, 0.1mol/L) is added for surface etching, then stirring and reacting are carried out for 30min at room temperature, and after the reaction is finished, the mixture is centrifuged to prepare brick red Cu with a nano hollow cubic structure2O base material, washing with distilled water several times, and then treating the nano hollow cubic junction by ultrasonic treatmentCu of structure2O base material was dispersed in ethanol (10mL) to form Cu2O dispersion liquid;
mixing 1ml of test solution containing Sudan red additive (different series) with 1ml of the above Cu2Mixing the O dispersion solutions, standing for 2h to reach adsorption balance, and respectively dripping 20 μ L of the mixed solution on clean Si/SiO2And naturally drying the substrate to obtain the sample plate 1 to be tested.
As shown in FIG. 1, it is Cu of the nano hollow cubic structure in the present embodiment2The enhanced Raman spectrogram of O as SERS active substrate with excitation wavelength of 785nm for different series of Sudan red probe molecules; 1136cm in the figure-1The absorption peaks are C-H and O-H in-plane vibration of naphthalene ring of Sudan red molecule, 1351cm-1Stretching vibration of the N ═ N bond corresponding to sudan red molecules.
Example 2
Under magnetic stirring, adding CuCl2(1mL, 0.1mol/L), NaOH solution (1mL, 2mol/L) and distilled water (40mL) are mixed, L-ascorbic acid (1mL, 0.1mol/L) is added for surface etching, then stirring reaction is carried out for 15min at room temperature, and after the reaction is finished, centrifugation is carried out to obtain brick red solid nano cube Cu2O；
Weighing 0.3mmol of solid nanocubes Cu after drying treatment2O, 0.2mmol of terephthalic acid and 0.4mmol of 4-4' bipyridyl are mixed, then 20ml of water and 20ml of ethanol are added, and the mixture is hydrothermally treated at 90 ℃ for 6 hours to prepare light blue MOF-Cu with a core-shell structure2O substrate material, then washing with ethanol several times, forming MOF-Cu by ultrasonic dispersion in ethanol2A dispersion of O.
1ml of a test solution containing Sudan Red additive (Sudan Red No. 3) was mixed with 1ml of the above MOF-Cu2Mixing O dispersion, standing for 2h to reach adsorption balance, and dripping 20 μ L of the mixed solution on clean Si/SiO2And naturally drying the substrate to obtain the sample plate 2 to be detected.
As shown in FIG. 2, it is MOF-Cu of core-shell structure in example 22Enhanced Raman spectrogram and excitation wave of O as SERS active substrate for Sudan Red Probe molecule (Sudan Red No. 3) with different concentrationsThe length is 785 nm;
example 3
Weighing 0.5g of powdery sample of chilli powder into a 50mL centrifuge tube, adding 10mL of ethanol, mixing for 1min, carrying out ultrasonic extraction for 30min, then centrifuging for 5min at 3000rpm, taking supernatant, diluting, adding Sudan red solutions with different proportions, standing overnight, fully mixing, taking 1mL of the mixed solution to be tested, mixing with 1mL of the base material dispersion liquid prepared in the embodiment 1, standing for 2h to achieve adsorption balance, taking 20 mu L of the mixed solution, and respectively dripping the mixed solution on clean Si/SiO2And naturally drying the substrate to obtain a sample plate 3 to be detected.
Example 4
Weighing 0.5g of tomato sauce sample in a 50mL centrifuge tube, adding 10-20mL of water to disperse the tomato sauce sample into paste, adding 10mL of ethanol to mix for 1min, carrying out ultrasonic extraction for 30min, centrifuging for 5min at 3000rpm, taking supernatant to dilute, adding Sudan red solutions with different proportions, standing overnight, fully mixing, taking 1mL of the mixed solution to be tested to mix with 1mL of the base material dispersion liquid prepared in the example 1, standing for 2h to achieve adsorption balance, taking 20 mu L of the mixed solution to drop into clean Si/SiO respectively2And naturally drying the substrate to obtain the sample plate 4 to be detected.
Example 5
Weighing 0.5g of capsicol sample in a 50mL centrifuge tube, adding 10mL of mixed solution of n-hexane and ethanol (the volume ratio of n-hexane to ethanol is 3:1), heating to promote dissolution, performing ultrasonic extraction for 30min, centrifuging at 3000rpm for 5min, diluting the supernatant, adding Sudan red solutions with different proportions, standing overnight, mixing completely, mixing 1mL of the mixed solution to be tested with 1mL of the base material dispersion prepared in example 1, standing for 2h to achieve adsorption balance, and dripping 20 mu L of the mixed solution in clean Si/SiO respectively2And naturally drying the substrate to obtain the sample plate 5 to be detected.
Example 6
Weighing 0.5g of crushed sausage in a 50mL centrifuge tube, adding 10mL of ethanol, fully homogenizing, carrying out ultrasonic extraction for 30min, centrifuging at 3000rpm for 5min, taking supernatant, diluting, adding Sudan red solutions in different proportions, standing overnight, fully mixing, taking 1mL of the mixed solution to be tested and 1mL of the base material prepared in the example 1Mixing the dispersion solutions, standing for 2h to reach adsorption balance, and dripping 20 μ L of the mixed solution on clean Si/SiO2And naturally drying the substrate to obtain the sample plate 6 to be tested.
FIG. 3 shows Cu of hollow nanocube structure in examples 3 to 6 of the present invention2And the enhanced Raman spectrogram of O serving as an SERS active substrate for chilli powder, tomato sauce, chili oil and sausage has the excitation wavelength of 785 nm.
Example 7
The preparation concentration is 10-4mixing equal parts of a mixed pigment solution of Sudan red, amaranth, carmine, sunset yellow and lemon yellow in mol/L, mixing 1ml of the obtained mixed solution to be tested with 1ml of the base material dispersion prepared in example 1, standing for 2h to achieve adsorption balance, and dripping 20 mu L of the mixed solution on clean Si/SiO2And naturally drying the substrate to obtain the sample plate 7 to be detected.
As shown in FIG. 4, it is Cu of the hollow cubic nanostructure in this example 72And the enhanced Raman spectrograms of the O substrate and the Ag sol to the mixed pigment molecules respectively have the excitation wavelength of 785 nm.
Comparative example 1
Mixing nano solid cubic Cu2O base material was dispersed in ethanol (10mL) to form Cu2O dispersion liquid;
mixing 1ml of Sudan red-containing solution to be tested with 1ml of the above Cu2Mixing the O dispersion solutions, standing for 2h to reach adsorption balance, and respectively dripping 20 μ L of the mixed solution on clean Si/SiO2Naturally drying the substrate to obtain a sample plate 8 to be detected;
FIGS. 5a to 5c are Cu of solid cubic structure in comparative example 1 of the present invention2O, Cu of nano hollow cubic structure prepared in example 12O (hollow cube Cu)2O), MOF-Cu of core-shell structure prepared in example 22An electron micrograph of O;
FIG. 6 shows Cu of nano hollow cubic structure prepared in example 1 of the present invention2O substrate and Cu of solid cubic structure prepared in comparative example 12O pair 10-4Enhanced Raman spectra of Sudan Red at mol/L concentration.
In addition, the inventors of the present invention have also made experiments with other materials, process operations, and process conditions described in the present specification with reference to the above examples, and have obtained preferable results.
The aspects, embodiments, features and examples of the present invention should be considered as illustrative in all respects and not intended to be limiting of the invention, the scope of which is defined only by the claims. Other embodiments, modifications, and uses will be apparent to those skilled in the art without departing from the spirit and scope of the claimed invention.
The use of headings and chapters in this disclosure is not meant to limit the disclosure; each section may apply to any aspect, embodiment, or feature of the disclosure.
Throughout this specification, where a composition is described as having, containing, or comprising specific components or where a process is described as having, containing, or comprising specific process steps, it is contemplated that the composition of the present teachings also consist essentially of, or consist of, the recited components, and the process of the present teachings also consist essentially of, or consist of, the recited process steps.
It should be understood that the order of steps or the order in which particular actions are performed is not critical, so long as the teachings of the invention remain operable. Further, two or more steps or actions may be performed simultaneously.
While the invention has been described with reference to illustrative embodiments, it will be understood by those skilled in the art that various other changes, omissions and/or additions may be made and substantial equivalents may be substituted for elements thereof without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from its scope. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed for carrying out this invention, but that the invention will include all embodiments falling within the scope of the appended claims. Moreover, unless specifically stated any use of the terms first, second, etc. do not denote any order or importance, but rather the terms first, second, etc. are used to distinguish one element from another.
Claims (10)
1. Application of copper-based semiconductor compound serving as SERS active substrate material in Sudan red specificity detection, wherein the copper-based semiconductor compound comprises Cu with a hollow structure2O-base material and/or MOF-Cu of core-shell structure2And (3) O base material.
2. The use according to claim 1, wherein the preparation method of the nano copper-based semiconductor compound comprises:
reacting a first mixed reaction system containing copper chloride, sodium hydroxide, a reducing agent and water at room temperature for 30min to prepare Cu with a hollow structure2An O base material;
or reacting a second mixed reaction system containing copper chloride, sodium hydroxide, a reducing agent and water at room temperature for 15min to obtain Cu with a solid structure2O; then making Cu containing the solid structure2Carrying out hydrothermal reaction on a third mixed reaction system of O, terephthalic acid, 4-4' bipyridine, ethanol and water at 90 ℃ for 6h to prepare the MOF-Cu with the core-shell structure2And (3) O base material.
3. Use according to claim 1, wherein the reducing agent comprises L-ascorbic acid and/or glucose, preferably L-ascorbic acid;
and/or, MOF-Cu of said core-shell structure2The core of the O substrate material is cuprous oxide, and the shell is MOF structure;
and/or, MOF-Cu of said core-shell structure2The grain diameter of the core in the O substrate material is 245-255nm, preferably 250 nm;
and/or, MOF-Cu of said core-shell structure2The thickness of the shell in the O substrate material is 100-200nm, preferably 150 nm;
and/or the molar concentration ratio of copper chloride, sodium hydroxide and a reducing agent in the first mixed reaction system is 1:1: 1;
and/or the molar concentration ratio of copper chloride, sodium hydroxide and a reducing agent in the second mixed reaction system is 1:20: 1;
and/or, Cu of solid structure in the third mixed reaction system2The molar ratio of O, terephthalic acid and 4-4' bipyridyl is 3:2: 4.
4. Use according to claim 1, characterized in that: the Sudan red comprises any one or combination of more than two of Sudan red No. 1, Sudan red No. 3, Sudan red B and Sudan red G.
5. The SERS active substrate material for detecting the specificity of Sudan red is characterized by comprising a nano copper-based semiconductor compound, wherein the nano copper-based semiconductor compound comprises Cu with a hollow structure2O-base material and/or MOF-Cu of core-shell structure2And (3) O base material.
6. The method for preparing a SERS-active substrate material for sudan red specific detection according to claim 5, comprising:
reacting a first mixed reaction system containing copper chloride, sodium hydroxide, a reducing agent and water at room temperature for 30min to prepare Cu with a hollow structure2An O base material;
or reacting a second mixed reaction system containing copper chloride, sodium hydroxide, a reducing agent and water at room temperature for 15min to obtain Cu with a solid structure2O; then making Cu containing the solid structure2Carrying out hydrothermal reaction on a third mixed reaction system of O, terephthalic acid, 4-4' bipyridine, ethanol and water at 90 ℃ for 6h to prepare the MOF-Cu with the core-shell structure2And (3) O base material.
7. The method according to claim 6, wherein the reducing agent comprises L-ascorbic acid and/or glucose, preferably L-ascorbic acid.
8. The preparation method according to claim 6, wherein the molar concentration ratio of the copper chloride to the sodium hydroxide to the reducing agent in the first mixed reaction system is 1:1: 1;
and/or the molar concentration ratio of copper chloride, sodium hydroxide and a reducing agent in the second mixed reaction system is 1:20: 1;
and/or, Cu of solid structure in the third mixed reaction system2The molar concentration ratio of O, terephthalic acid and 4-4' bipyridyl is 3:2: 4.
9. A method for detecting the specificity of Sudan red is characterized by comprising the following steps:
the method comprises the following steps of (1) taking a nano copper-based semiconductor compound as an SERS active substrate material; or providing the SERS-active substrate material of claim 5;
and contacting the SERS active substrate material with a detection sample possibly containing Sudan red, and detecting by using a Raman spectrometer to realize the specific detection of the Sudan red.
10. The method for the specific detection of sudan red according to claim 9, wherein: the Sudan red comprises any one or combination of more than two of Sudan red No. 1, Sudan red No. 3, Sudan red B and Sudan red G.
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Inventor after: Cong Shan Inventor after: Zhang Taoyang Inventor after: Jiang Yuxiao Inventor after: Zhao Zhigang Inventor before: Zhao Zhigang Inventor before: Zhang Taoyang Inventor before: Jiang Yuxiao Inventor before: Cong Shan |
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| CB03 | Change of inventor or designer information |