CN108344726A - A kind of 2,4 dichlorophenoxyacetic acid based on gold nanometer film SERS technologies(2,4-D)The detection method of pesticide - Google Patents
A kind of 2,4 dichlorophenoxyacetic acid based on gold nanometer film SERS technologies(2,4-D)The detection method of pesticide Download PDFInfo
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- 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
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Abstract
The detection method of the invention discloses a kind of 2,4 dichlorphenoxyacetic acids (2,4 D) pesticide based on gold nanometer film SERS technologies, belongs to the technical fields such as Food Monitoring.Pass through the Photoinduced Reduction generation gold nano grain in situ on the mesoporous silica film that air-water interface is formed first, build the gold nano surface enhanced Raman substrate of meso-hole structure, compact arranged gold nano grain and 2 in film, Raman signal is enhanced after 4 D molecule Electrostatic Absorptions, establish the standard curve of 2,4 D detections.This method is easy to operate, and detection speed is fast, precision is higher, stability is good, can realize in situ detection to 2,4 D pesticides.
Description
Technical field
Invention describes a kind of 2,4 dichlorophenoxyacetic acid (2,4-D) pesticide based on gold nanometer film SERS technologies
Detection method is prepared for the surface Raman enhancement substrate of orderly gold nanometer film to enhance pesticide 2, and the Raman signal of 4-D uses
Density function theory pesticide 2, the theoretical Raman spectrum of 4-D establish the standard curve that 2,4-D pesticides quantitatively detect.This
Inventive method is easy to operate, and detection speed is fast, precision is higher, stability is good etc. may be implemented to the inspection in situ of the high-volume of 2,4-D
It surveys.This method is suitable for the technical fields such as food security, materials chemistry.
Background technology
2,4 dichlorophenoxyacetic acid (2,4-D) is representative synthetic auxin and a kind of main weeding
Agent, it is also possible to make plant growth regulation, be one kind of the common auxin analog formed for evoked callus.Such as
The excessive use 2,4-D of fruit, due to its strong adsorption, residual minim medicament can cause certain harm, and application method is improper, then
The toxic side effect that people can be caused different with livestock degree.Harmful pesticide residue is not only closely related with national personal safety,
And an important factor for having become influence China's milk foreign trade.Therefore, the residual detection importance of agriculture becomes increasingly conspicuous, right
It is analyzed testing result and shows higher target.The detection of agriculture residual limit standard and cumulative year after year that countries in the world reduce year by year
Project shows higher requirement to its analyzing detecting method, and conventional the Detection Technologies of Pesticide Residues is in analyte detection process
There are many defects, especially in sensitivity, accuracy, testing cost, detection time limit etc..Therefore, research it is a kind of efficiently,
Accurately, sensitive modern residue detection means are of great significance.The conventional detection side for pesticide 2,4-D at present
Method mainly has immuno analytical method, instrument analysis technology, spectral analysis technique.
Immuno analytical method is simple, sensitive, plays an important roll in farming residual analysis detection.Most common method has:Enzyme
Immunological technique, radioimmunoassay technique and golden immunological technique.Immunoenzyme techniques (Enzyme immunoassay, EIA) are mainly used
Enzyme is marked, and is connect with antigen (or antibody) after labeled, makes antibody and enzyme-labelled antigen knot using the specific reaction of the two
It closes (or antigen is combined with enzyme labelled antibody), reaction substrate is then added, carried out by the chromogenic reaction of enzyme and respective reaction object
The qualitative and quantitative analysis of determinand.Radioimmunoassay technique (Radioimmunoassay, RIA) is that one kind combining high sensitivity
Radioisotopic tracer and high degree of specificity antigen/precursor reactant, pass through and object letter obtained to the tracking of isotope
The detection and analysis of breath.Golden immunological technique (Immune colloidalgold labeling technique, ICG) mainly utilizes
The high density that gold particle has makes its existing stain under the only instrument amplification of the junction of golden labelled protein, and matches corresponding
At body can bore hole regard powder (red) point, so can be used for qualitative and half-quantitative detection.Pesticide residue inspection based on immuno analytical method
Survey method can reduce the use of poisonous and harmful reagent, keep detection operation succinct, have higher reaction sensitivity, but still
There are some disadvantages, such as enzyme viability to be limited in scope, and causes the scope of application for detecting object limited, the use of antigen-antibody
Cost is higher etc..
Instrument analysis technology, it is main at present with using gas chromatography, high performance liquid chromatography, gas chromatography-mass spectrography and
Liquid chromatography-mass spectrometry carries out the detection of pesticide residue.Gas chromatography (Gas Chromatography, GC) is mainly foundation
Gas phase and the different target spot properties of stationary phase and its difference of breadth coefficient, make Multiple Pesticides between gas and solid two-phase
Repeatedly distribution, to realize the separation of target detection object, finally sequentially into ranks, separation.High performance liquid chromatography
Method (High Performance Liquid Chromatography, HPLC) is to build on Traditional liquid phase chromatography, and merge gas
The related mechanism and technology of phase chromatography, to detect and quantify a kind of modern separate analytical technique of heterogeneity ratio.Gas phase
Chromatography-mass spectroscopy (Gas Chromatography-Mass Spectrometry, GC-MS) is a kind of by gas chromatograph and mass spectrum
As a whole, wherein GC is used for the ingredient in separating mixture to instrument;MS's act as the molecular weight to unknown compound, divides
Minor or functional group are identified.Liquid chromatography-mass spectrometry (Liquid Chromatography-Mass Spectrometry,
LC-MS) it is a kind of analysis method using liquid chromatograph and mass spectrograph as a whole.Upper the method analysis ability
By force, detection range is wide, and result has the features such as reliable and stable, high sensitivity and favorable reproducibility, and mature is formed centainly
Professional standard, but its pre-treatment step is complicated and detection process is complicated, instrument and equipment is expensive, analysis time is very long, and specificity is not
Obviously, and need professional operator's auxiliary that could complete analysis detection.Therefore, it is not suitable with the quick detection at scene, it is also unfavorable
The purpose of Fast Determination of Pesticide Residue in popularization and application and realization milk.
In recent years, with the fast development of technical device, a series of spectrum analysis detection methods are come into being.It leads herein
Domain, the Detection Technologies of Pesticide Residues being commonly used at present include:High light spectrum image-forming, fluorescence spectrum, FT-IR & FT-RAMAN spectra.
Compared with traditional analyzing detecting method, spectroscopic analysis methods have the characteristics that quick, easy, environmental protection, can be used for pesticide residue
Quick detection, for pesticide in milk it is remaining detection provide some new solutions.But meanwhile they there is also certain
Deficiency, be still weak in terms of the precision of quantitative analysis and sensitivity.Such as hyperspectral technique and infrared spectrum technology try
The spectrum statistical nature for having tested pesticide, is suitable for the Pesticides Testing of higher concentration, and for micro or trace pesticide residue
Detection result has much room for improvement;Light spectral technique makes it equally be deposited in application range because some pesticides do not have fluorescent characteristic
In certain limitation.
Surface enhanced Raman spectroscopy (Surface-Enhanced Raman Scattering, SERS) technology is Raman light
The extension of spectrum with it is perfect.Its spectrum can obtain the finger print information of molecular structure, have powerful molecule distinguishability, be molecule
The promising approach of information quick obtaining.Therefore, quick, Sensitive Detection sensing of the surface-enhanced Raman method in structure trace materials
In terms of device, prodigious concern and application have been obtained.According to the Raman peak intensity under measured object specific wavelength, measured object can be established
Linear relationship between concentration and Raman peak intensity realizes the quantitative analysis to measured object concentration.In the recent period, studies have shown that metal
There are certain contacts between nanometer and " Raman hot spot " between nano-particle, and it was found that when interparticle distance reduces
When, the intensity of SERS will greatly enhance i.e. we can be adjusted using the reinforcement of the phasmon coupled electromagnetic field between particle
Whole SERS signal carries out simple homogeneous determination experiment to realize under the premise of remaining highly sensitive.It is produced by the present invention
SERS substrates have close orderly meso-hole structure, so that the spacing between gold nanoparticle is reduced, while also preventing
Having stopped reduces detectability because of agglomeration between gold nano, to improve the stability of detection pesticide and sensitive
Property.
Invention content
The object of the present invention is to provide a kind of 2,4 dichlorophenoxyacetic acid (2,4-D) based on gold nanometer film SERS technologies
The detection method of pesticide, high sensitivity, highly reliable, detection speed is fast, realizes the quick label-free inspection of 2,4-D pesticides
It surveys.
To achieve the goals above, technical scheme of the present invention includes:The preparation of air-water interface mesoporous silicon oxide,
The photoinduction of AuNP assembles, and various concentration sample surfaces enhance the acquisition of Raman spectrum SERS, establishes standard curve, realizes 2,4-
The quantitative detection of D pesticides.This method is suitable for the technical fields such as food security, environmental monitoring.
A kind of detection side of above-mentioned 2,4 dichlorophenoxyacetic acid (2,4-D) pesticide based on gold nanometer film SERS technologies
Method the gold nanometer film of ordered arrangement is made with the method for simple self assembly, photoinduction and in-situ reducing, in conjunction with Raman spectrum
Technology is built to pesticide 2, the quantitative detection architecture of 4-D.Specifically include following steps:
The preparation of step 1) air-water interface mesoporous silicon oxide:In aqueous hydrochloric acid solution in acid condition, by 16
Stirring and dissolving takes after above-mentioned mixed solution stirs evenly successively for alkyl trimethyl ammonium bromide, tetramethoxy-silicane and tungstophosphoric acid
Certain volume morning solution is put into culture dish and the sealing that closes the lid, after standing a period of time under room temperature environment, in air-
The interface of water grows to obtain transparent film;
The assembling of step 2) AuNP:A certain amount of HAuCl is injected under above-mentioned mesoporous silica film4, stand one section
After time, film becomes faint yellow, and after being radiated with ultraviolet lamp, film becomes lavender.The lavender film glass that will be obtained
Piece is gently chosen, and after being cleaned for several times with deionized water, is dried at room temperature for, and obtains mesoporous gold nanometer film;
Step 3) sample surfaces enhance the acquisition of Raman spectrum SERS:Pesticide 2,4-D is detected using label-free method
Raman characteristic peak, and compared with the theoretical raman spectra of the calculating of density functional theory, realize Characteristic Raman spectrum
The ownership at peak, to further establish the standard curve between Raman signal intensity and corresponding pesticide concentration.
Further, the detailed process of the step 1) is the preparation of air-water interface mesoporous silicon oxide:In ph<2
In aqueous hydrochloric acid solution, by cetyl trimethylammonium bromide, tetramethoxy-silicane and tungstophosphoric acid successively stirring and dissolving, when above-mentioned mixed
After conjunction solution stirs evenly, takes 30ml to be put into culture dish and the sealing that closes the lid, stood for 24 hours in the environment of 25 degrees Celsius
Afterwards, it grows to obtain transparent film in the interface of Air-Water.
Further, in the step 1), the method that independently filled using air-water interface has synthesized mesoporous with meso-hole structure
Silica membrane is used for load gold nano grain.
Further, the detailed process of the step 2) is:Inject a certain amount of 5mM's under above-mentioned mesoporous silica film
HAuCl4, after standing 30min, film becomes faint yellow, and after the ultraviolet lamp radiation 3h of 254nm, film becomes lavender.Will
To lavender film sheet glass gently choose, after being cleaned for several times with deionized water, be dried at room temperature for, obtain mesoporous Jenner
Rice film.
Further, in the step 2), using ion exchange combination photoinduction mode, make gold nano grain in mesoporous dioxy
Synthesis in situ is carried out in the duct of SiClx.
Further, in the step 2), using the HAuCl of 5mM4Meso-porous titanium dioxide silicon base of the solution to load gold nano
In-situ reducing is carried out, the raman spectrum strength of sample is enhanced.
Further, it in the step 3), weighs a certain amount of gold nanometer film substance and is mixed respectively with 2,4-D of various concentration
One hour, under 780nm laser excitations, Raman spectrum is acquired using the Portable Raman spectrometer voluntarily built, to establish
Standard curve between Raman signal intensity and corresponding 2,4-D concentration is applied in actual sample detection.
Further, in the step 3), gold nanometer film is synthesized for template load gold nano using mesoporous silicon oxide
As surface Raman enhancement substrate.
Further, in the step 3), pesticide 2,4-D is detected using label-free method, is produced with aptamers are connect
The detection method of raw specific reaction is compared.
Compared with prior art, the advantage of the invention is that:
1) surface enhanced Raman substrate prepared by the present invention, using ordered mesoporous silica dioxide combination gold nano grain conduct
Surface Raman enhancement substrate.
2) surface enhanced Raman substrate prepared by the present invention has since gold nano grain is grown in meso-hole structure
Effect prevents gold nano grain to generate stability and sensitivity that agglomeration affects detection due to long-time storage
Phenomenon generates.
3) present invention detects 2,4-D pesticides using non-marked method, saves testing cost, improves detection speed.
4) detection method prepared by the present invention can be used for the in situ detection of various small molecule pesticides in food, detection speed
Degree is fast, and detection range is wide, stability, high sensitivity, in the technical fields extensive use such as food security, environmental monitoring.
Description of the drawings
Fig. 1 is the phenogram of gold nanometer film:(A) it is characterized for the transmission electron microscope of gold nanometer film;(B) it is gold nanometer film
The average grain diameter figure of middle gold nanoparticle.
Fig. 2 is the Surface enhanced Raman spectroscopy figure of various concentration 2,4-D pesticides.
Fig. 3 is the canonical plotting of various concentration 2,4-D pesticides.
Specific implementation mode
Embodiment 1 is in order to further verify detection of the detection method prepared by the present invention to food small molecular pesticide
Effect, present example, by taking the detection of 2,4-D pesticides in milk as an example, concrete operation step is as follows:
1) preparation of air-water interface mesoporous silicon oxide:In ph<In 2 aqueous hydrochloric acid solution, by cetyl trimethyl
Stirring and dissolving takes 30ml to be put into training after above-mentioned mixed solution stirs evenly successively for ammonium bromide, tetramethoxy-silicane and tungstophosphoric acid
Support ware in and the sealing that closes the lid, after standing for 24 hours in the environment of 25 degrees Celsius, grow to obtain in the interface of Air-Water
Bright film.
2) assembling of AuNP:The HAuCl of a certain amount of 5mM is injected under above-mentioned mesoporous silica film4,Stand 30min
Afterwards, film becomes faint yellow, and after the ultraviolet lamp radiation 3h of 254nm, film becomes lavender.Obtained lavender film is used
Sheet glass is gently chosen, and after being cleaned for several times with deionized water, is dried at room temperature for, and obtains mesoporous gold nanometer film.
3) acquisition of sample surfaces enhancing Raman spectrum SERS:Weigh a certain amount of gold nanometer film substance respectively in milk
2,4-D of various concentration is mixed one hour, under 780nm laser excitations, is adopted using the Portable Raman spectrometer voluntarily built
Collect Raman spectrum, to establish the standard curve between Raman signal intensity and corresponding 2,4-D concentration, be applied to the 2 of mark-on sample,
In 4-D Pesticides Testing.
Table 1 is the testing result of 2,4-D in practical milk sample
To sum up, a kind of 2,4- dichlorphenoxyacetic acids (2,4-D) pesticide based on gold nanometer film SERS technologies of the invention
Detection method, belong to the technical fields such as Food Monitoring.Mesoporous silica film first by being formed in air-water interface
Upper original position Photoinduced Reduction generates gold nano grain, builds the gold nano surface enhanced Raman substrate of meso-hole structure, tight in film
The gold nano grain and 2 of solid matter row, enhances Raman signal after 4-D molecule Electrostatic Absorptions, establishes the standard song of 2,4-D detections
Line.This method is easy to operate, and detection speed is fast, precision is higher, stability is good, can realize in situ detection to 2,4-D pesticides.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " illustrative examples ",
The description of " example ", " specific example " or " some examples " etc. means specific features described in conjunction with this embodiment or example, knot
Structure, material or feature are included at least one embodiment or example of the invention.In the present specification, to above-mentioned term
Schematic representation may not refer to the same embodiment or example.Moreover, specific features, structure, material or the spy of description
Point can be combined in any suitable manner in any one or more of the embodiments or examples.
Although an embodiment of the present invention has been shown and described, it will be understood by those skilled in the art that:Not
In the case of being detached from the principle of the present invention and objective a variety of change, modification, replacement and modification can be carried out to these embodiments, this
The range of invention is limited by claim and its equivalent.
Claims (10)
1. a kind of detection method of 2,4- dichlorphenoxyacetic acids (2,4-D) pesticide based on gold nanometer film SERS technologies, special
Sign is:The gold nanometer film of ordered arrangement is made with the method for simple self assembly, photoinduction and in-situ reducing, in conjunction with Raman
Spectral technique is built to pesticide 2, the quantitative detection architecture of 4-D.
2. a kind of 2,4 dichlorophenoxyacetic acid (2,4-D) based on gold nanometer film SERS technologies according to claim 1
The detection method of pesticide, which is characterized in that specifically include following steps:
The preparation of step 1) air-water interface mesoporous silicon oxide:In aqueous hydrochloric acid solution in acid condition, by cetyl
Stirring and dissolving takes certain after above-mentioned mixed solution stirs evenly successively for trimethylammonium bromide, tetramethoxy-silicane and tungstophosphoric acid
Volume morning solution is put into culture dish and the sealing that closes the lid, after standing a period of time under room temperature environment, in Air-Water
Interface grows to obtain transparent film;
The assembling of step 2) AuNP:A certain amount of HAuCl is injected under above-mentioned mesoporous silica film4, stand a period of time
Afterwards, film becomes faint yellow, and after being radiated with ultraviolet lamp, film becomes lavender.Obtained lavender film sheet glass is light
Gently choose, after being cleaned for several times with deionized water, be dried at room temperature for, obtains mesoporous gold nanometer film;
Step 3) sample surfaces enhance the acquisition of Raman spectrum SERS:The drawing of pesticide 2,4-D is detected using label-free method
Graceful characteristic peak, and compared with the theoretical raman spectra of the calculating of density functional theory, realize Characteristic Raman spectral peak
Ownership, to further establish the standard curve between Raman signal intensity and corresponding pesticide concentration.
3. a kind of 2,4 dichlorophenoxyacetic acid (2,4-D) based on gold nanometer film SERS technologies according to claim 2
The detection method of pesticide, which is characterized in that the detailed process of the step 1) is the system of air-water interface mesoporous silicon oxide
It is standby:In ph<In 2 aqueous hydrochloric acid solution, cetyl trimethylammonium bromide, tetramethoxy-silicane and tungstophosphoric acid are stirred successively molten
Solution, after above-mentioned mixed solution stirs evenly, takes 30ml to be put into culture dish and the sealing that closes the lid, in 25 degrees Celsius of environment
It is lower standing for 24 hours after, grow to obtain transparent film in the interface of Air-Water.
4. a kind of 2,4 dichlorophenoxyacetic acid (2,4-D) based on gold nanometer film SERS technologies according to claim 2
The detection method of pesticide, which is characterized in that in the step 1), the method that independently filled using air-water interface has been synthesized with Jie
The mesoporous silica film of pore structure is used for load gold nano grain.
5. a kind of 2,4 dichlorophenoxyacetic acid (2,4-D) based on gold nanometer film SERS technologies according to claim 2
The detection method of pesticide, which is characterized in that the detailed process of the step 2) is:It is injected under above-mentioned mesoporous silica film
The HAuCl of a certain amount of 5mM4, after standing 30min, film becomes faint yellow, and after the ultraviolet lamp radiation 3h of 254nm, film becomes
Lavender.Obtained lavender film sheet glass is gently chosen, after being cleaned for several times with deionized water, is dried at room temperature for,
Obtain mesoporous gold nanometer film.
6. a kind of 2,4 dichlorophenoxyacetic acid (2,4-D) based on gold nanometer film SERS technologies according to claim 2
The detection method of pesticide, which is characterized in that in the step 2), using ion exchange combination photoinduction mode, make gold nano
Grain carries out synthesis in situ in the duct of mesoporous silicon oxide.
7. a kind of 2,4 dichlorophenoxyacetic acid (2,4-D) based on gold nanometer film SERS technologies according to claim 2
The detection method of pesticide, which is characterized in that in the step 2), using the HAuCl of 5mM4Solution is to the mesoporous of load gold nano
Silica substrate carries out in-situ reducing, enhances the raman spectrum strength of sample.
8. a kind of 2,4 dichlorophenoxyacetic acid (2,4-D) based on gold nanometer film SERS technologies according to claim 2
The detection method of pesticide, which is characterized in that in the step 3), weigh a certain amount of gold nanometer film substance respectively and various concentration
2,4-D mix one hour, under 780nm laser excitations, utilize voluntarily build Portable Raman spectrometer acquisition Raman light
Spectrum is applied to establish the standard curve between Raman signal intensity and corresponding 2,4-D concentration in actual sample detection.
9. a kind of 2,4 dichlorophenoxyacetic acid (2,4-D) based on gold nanometer film SERS technologies according to claim 2
The detection method of pesticide, which is characterized in that in the step 3), synthesized for template load gold nano using mesoporous silicon oxide
Gold nanometer film is as surface Raman enhancement substrate.
10. a kind of 2,4 dichlorophenoxyacetic acid (2,4-D) based on gold nanometer film SERS technologies according to claim 2
The detection method of pesticide, which is characterized in that in the step 3), pesticide 2,4-D is detected using label-free method, and is connect
Aptamers are compared to generate the detection method of specific reaction.
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Cited By (2)
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CN109470683A (en) * | 2018-10-23 | 2019-03-15 | 江苏大学 | A method of 2,4-D is carried out with SERS substrate combination multiple linear regression model and is quickly detected |
CN109752363A (en) * | 2019-02-28 | 2019-05-14 | 江苏大学 | The remaining Portable Raman optical spectrum detection method of pesticide in a kind of instant tea powder |
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CN107044974A (en) * | 2017-03-28 | 2017-08-15 | 北京工业大学 | 2,4 dichlorphenoxyacetic acid method for detecting residue in a kind of fruits and vegetables |
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CN107044974A (en) * | 2017-03-28 | 2017-08-15 | 北京工业大学 | 2,4 dichlorphenoxyacetic acid method for detecting residue in a kind of fruits and vegetables |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109470683A (en) * | 2018-10-23 | 2019-03-15 | 江苏大学 | A method of 2,4-D is carried out with SERS substrate combination multiple linear regression model and is quickly detected |
CN109752363A (en) * | 2019-02-28 | 2019-05-14 | 江苏大学 | The remaining Portable Raman optical spectrum detection method of pesticide in a kind of instant tea powder |
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