CN107037214B - The residual detection sensor preparation method of agriculture based on hollow optical fiber - Google Patents
The residual detection sensor preparation method of agriculture based on hollow optical fiber Download PDFInfo
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Abstract
The present invention relates to the residual detection technique field of agriculture, the residual detection sensor preparation method of more particularly to a kind of agriculture based on hollow optical fiber includes the following steps：(A) using nano-particle as substrate, nano artificial antibody of the synthesis with the pesticide molecule marking；(B) the Nanometer core shell particles that fluorescent marker acquisition has fluorescence labelling and the pesticide molecule marking concurrently are carried out to nano artificial antibody；(C) Nanometer core shell particles are assembled in the inner surface of hollow optic fibre.It is residual that sensor made of this method can be good at detection agriculture, by carrying out the pesticide molecule marking to nano-particle, it can solve the problems, such as selective enrichment and identification of the nano material to pesticide molecule, the combination of target pesticide molecule is converted to exportable sensitive fluorescent signal by fluorescence labelling, by carrying out spectrum analysis to fluorescence signal, with regard to that can obtain corresponding pesticide molecule residual quantity information, while this method step is simple, favorable repeatability, and the production cost of sensor can be greatly reduced and improve yield.
Description
Technical field
The present invention relates to the residual detection technique field of agriculture, the residual detection sensor system of more particularly to a kind of agriculture based on hollow optical fiber
Preparation Method.
Background technology
Pesticide using playing huge effect for the use of ensureing that higher yield of crops increases income, but excessive, unreasonable agriculture
Medicine application brings persistent pollution to China's agricultural environment, the ecosystem is caused to be difficult to the destruction made up, pesticide is in agriculture
Residual in product is food-safe and life and health has formed direct threat, however, progress high selection residual to agriculture, high throughput
On-line checking is still a challenge.The main method of Detecting Pesticide has：Gas chromatography, liquid chromatography, mass spectrography
Deng, these method high sensitivities, but required instrument is generally laboratory large-scale instrument, price costly, and is difficult to apply
In the online detection in scene.
In recent years, there is many effective discriminatings and analyzing detecting method, mainly have following several：The first,
Immune bio-sensing method, this method arrange the amino acid molecular formed as antibody by the use of high-sequential, can be with agriculture according to it
Medicine molecular antigen height exclusively Reversible binding, realizes the quick detection residual to agriculture；However, biological antibody material source is limited,
Service life is short, may lose sensitivity characteristic under severe conditions.Second, enzyme inhibition, this method inhibits principle using enzyme
Electrochemical sensing and fluorescence probe can be made；Enzyme inhibition major defect has：Enzyme inhibition is disturbed greatly, and selectivity is low；
Organophosphor and enzyme it is irreversible binding affinity strong, enzyme is suppressed rear difficult life；The influence of temperature, acid-base property to enzyme is big.The third, changes
Luminescence analysis is learned, this method has many advantages, such as range of linearity is wide, instrument and equipment is simple, analysis is quick, utilizes chemistry
Luminescence method has realized the detection to pesticide residues such as organic phosphates, carbamates, but chemiluminometry poor selectivity
Seriously limit its application development.4th kind, Surface enhanced Raman scattering, this method have very strong fingerprint recognition characteristic, it is lossless,
The advantages that sample aequum is small, the existing document report enhancing Raman detection residual to agriculture at present, however the reliability of Raman detection
With the development for repeating sex chromosome mosaicism influence and restricting its application.Above method is also mainly laboratory analysis technique and hand at present
Section, it is difficult to meet environment selectivity residual with agricultural product middle peasant, high-throughput online or Site Detection demand.
Invention content
The purpose of the present invention is to provide a kind of residual detection sensor preparation methods of agriculture based on hollow optical fiber, can repeat
Prepare high selection, the high-throughput residual detection sensor of agriculture.
In order to achieve the above object, the technical solution adopted by the present invention is：A kind of residual detection sensing of agriculture based on hollow optical fiber
Device preparation method, includes the following steps：(A) using nano-particle as substrate, nano artificial of the synthesis with the pesticide molecule marking resists
Body；(B) the Nanometer core shell particles that fluorescent marker acquisition has fluorescence labelling and the pesticide molecule marking concurrently are carried out to nano artificial antibody；
(C) Nanometer core shell particles are assembled in the inner surface of hollow optic fibre.
Compared with prior art, there are following technique effects by the present invention：Sensor made of this method can be good at examining
It is residual to survey agriculture, by carrying out the pesticide molecule marking to nano-particle, selective enrichment of the nano material to pesticide molecule can be solved
The problem of with identification, the combination of target pesticide molecule is converted to exportable sensitive fluorescent signal by fluorescence labelling, by glimmering
Optical signal carries out spectrum analysis, and with regard to that can obtain corresponding pesticide molecule residual quantity information, while this method step is simple, repeatable
Property is good, and the production cost of sensor can be greatly reduced and improve yield.
Description of the drawings
Fig. 1 is the nano artificial antibody composition principle figure for having the pesticide molecule marking；
Fig. 2 is the schematic diagram that fluorescence labelling is carried out in nano artificial antibody building-up process；
Fig. 3 is Nanometer core shell particles in hollow optical fiber inner surface assembling schematic diagram.
Specific embodiment
With reference to Fig. 1 to Fig. 3, the present invention is described in further detail.
Refering to Fig. 1-3, a kind of residual detection sensor preparation method of agriculture based on hollow optical fiber includes the following steps：(A) with
Nano-particle is substrate, nano artificial antibody of the synthesis with the pesticide molecule marking；(B) fluorescence mark is carried out to nano artificial antibody
Note obtains the Nanometer core shell particles for having fluorescence labelling and the pesticide molecule marking concurrently；(C) Nanometer core shell particles are assembled in hollow light
Fine inner surface.It is residual that sensor made of this method can be good at detecting agriculture, by carrying out pesticide point to nano-particle
The sub- marking, can solve the problems, such as selective enrichment and identification of the nano material to pesticide molecule, and fluorescence labelling is by target pesticide
The combination of molecule is converted to exportable sensitive fluorescent signal, corresponding with regard to that can obtain by carrying out spectrum analysis to fluorescence signal
Pesticide molecule residual quantity information, while this method step is simple, favorable repeatability, and the production cost of sensor can be greatly reduced
And improve yield.When preparing sensor, according to the difference of pesticide molecule structure, suitable step can be selected to nano-particle
Carry out the pesticide molecule marking.
There are many kinds of nano-particles, such as silica, titanium dioxide, gold and silver particle, a variety of quantum dots, magnetic particle,
Structure type includes nano wire, nanotube, nanosphere, nano-hollow particle and Nanometer core shell particles etc., due to silica material
Have many advantages, such as that rigidity is strong, the retentivity of binding site is good, easy progress functional modification, particularly suitable for being passed in chemical-biological
The artificial antibody's material applied in terms of sensor, therefore nano-particle here can preferably prepare relatively easy silica nanometer
Particle is as substrate.
Refering to Fig. 1, according to different pesticide molecules, the step of pesticide molecule marking is carried out to nano-particle and add in anti-
Solvent is answered all to be not quite similar, two kinds of embodiments are provided here, respectively to heterocyclic pesticide molecule (such as fenifrothion
Fenitrothion) and 2,4- dichlorphenoxyacetic acid organo-chlorine pesticide carry out the pesticide molecule marking, the marking of other pesticide molecules
The two schemes can be referred to.
Embodiment one：The pesticide molecule is heterocyclic pesticide molecule, and step A synthesizes nano artificial and resists as follows
Body：(A11) nano-particle with hydroxyl is selected as substrate；(A12) aminopropyl triethoxysilane and nano-particle are utilized
On hydroxyl alcoholysis reaction occurs and by the aminopropyl modification in aminopropyl triethoxysilane to nanoparticle surface；(A13)
Heterocyclic pesticide molecule is added in, between the aminopropyl of electron rich and the heterocyclic pesticide molecule of electron deficient there is strong electric charge transfer to make
With and form relatively stable APTS- heterocyclic pesticide molecular complexes；(A14) it is crosslinking using ethylene glycol dimethacrylate
Agent is cured by APTS- heterocyclic pesticides molecular complex after heating polymerization；(A15) pass through extraction, acidolysis or chemical reaction
Heterocyclic pesticide template molecule is removed, obtains the nano artificial antibody with heterocyclic pesticide molecular imprinting.
Embodiment two：The pesticide molecule is organo-chlorine pesticide molecule, and step A synthesizes nano artificial as follows
Antibody：(A21) nano-particle with hydroxyl is selected as substrate；(A22) aminopropyl triethoxysilane and nanoparticle are utilized
Hydroxyl on son occurs alcoholysis reaction and modifies the aminopropyl in aminopropyl triethoxysilane to nanoparticle surface；
(A23) acetate buffer is added in, by aldehyde group modified to nanoparticle surface；(A24) 2,4 dichlorophenoxyacetic acid organochlorine is added in
Pesticide obtains APTS- organo-chlorine pesticide molecular complexes by electric charge transfer；(A25) ethylene glycol dimethacrylate is utilized
For crosslinking agent, cured by APTS- organo-chlorine pesticides molecular complex after heating polymerization；(A26) by extraction, acidolysis or
Organo-chlorine pesticide template molecule is removed in chemical reaction, obtains the nano artificial antibody with organo-chlorine pesticide molecular imprinting.
In above-mentioned two embodiment, basic principle is all first pesticide molecule to be attached on nano-particle, then by each
Physically or chemically means remove pesticide template molecule to kind, you can leave the pesticide molecule marking.During the reaction, it is tried by controlling
Agent concentration and dosage, solation temperature, soaking time and the conditions such as gelation and aging temperature can be formed to be combined with high
The nano artificial antibody material of capacity, highly selective, pattern and structure control.
Referring to Fig.2, by forming the pesticide molecule marking on nano-particle, the acquisition of pesticide molecule can be realized, in order to
Collected information is easily converted into the light easily identified, electric signal, continues to carry out fluorescence to nano artificial antibody here
Mark.By introducing the fluorescein molecule containing isothiocyanic acid in the nano artificial antibody with the pesticide marking come real in this case
The fluorescent marker of existing nano artificial antibody for being marked using fluorescent dye, is based primarily upon the anti-of amino and isothiocyanic acid
Should, fluorescent marker can be carried out to nano artificial antibody by two kinds of basic modes here：Mode one, in the step B,
Nanometer core shell particles are obtained as follows：(B1) using on the amino and fluorescein molecule on aminopropyl triethoxysilane
Active group isothiocyanic acid coupling reaction, form the new FITC-APTS function precursors with illuminophore；(B2) pass through
The polymerisation of FITC-APTS functions precursor and the pesticide molecule marking has fluorescence labelling and the pesticide molecule marking concurrently to directly obtain
Nanometer core shell particles.Nano artificial antibody material micropore inner surface in the step B, is carried the ammonia of part by mode two
Base is reacted with the fluorescent molecular containing active isothiocyano to being obtained after synthetic nano artificial antibody progress fluorescence labelling
To Nanometer core shell particles.
Refering to Fig. 3, in view of hollow-core photonic crystal fiber has the following advantages：It is the transmission of major diameter endless single mode, fabulous non-
Linear effect and birefringence effect, higher power transmission capabilities, are easily achieved multicore transmission at excellent chromatic dispersion performance,
Therefore preferably the Nanometer core shell particles for having fluorescence labelling and the pesticide molecule marking concurrently are modified to hollow photon crystal in the present invention
The inner surface of optical fiber, it is of course also possible to which other is selected suitably to be modified material.In the step C, as follows into
Row assembling：(C1) carrying out hydrophilic treated to optical fiber inner surface by the concentrated sulfuric acid and hydrogen peroxide makes its surface contain more hydroxyl；
(C2) optical fiber inner surface amination is made by aminopropyl triethoxysilane；(C3) using the glyoxal of both ends activity to hollow light
Fine inner surface carries out aldehyde group modified；(C4) glyoxal being not bound with fully is washed, since glyoxal is a kind of crosslinking agent, can be made
Reunion is generated containing amido modified nano artificial antibody, therefore should need fully to wash after optical fiber surface is modified and not have
There is the glyoxal of combination；(C5) Nanometer core shell particles, amino and the glyoxal suspension of Nanometer core shell particles surface residual are added in
Aldehyde radical is mutually bonded is made sensor so as to which Nanometer core shell particles are assembled into hollow optical fiber inner surface.The step can be realized and be had concurrently
The Nanometer core shell particles of fluorescence labelling and the pesticide molecule marking are self-assembled on the inner surface of hollow-core photonic crystal fiber, are realized
Come very convenient.
Claims (1)
1. a kind of residual detection sensor preparation method of agriculture based on hollow optical fiber, includes the following steps：
(A) using nano-particle as substrate, nano artificial antibody of the synthesis with the pesticide molecule marking；
(B) the Nanometer core capsomere that fluorescent marker acquisition has fluorescence labelling and the pesticide molecule marking concurrently is carried out to nano artificial antibody
Son；
(C) Nanometer core shell particles are assembled in the inner surface of hollow optic fibre；
If the pesticide molecule is heterocyclic pesticide molecule, step A synthesizes nano artificial antibody as follows：
(A11) nano-particle with hydroxyl is selected as substrate；
(A12) using the hydroxyl on aminopropyl triethoxysilane and nano-particle occur alcoholysis reaction and by three ethoxy of aminopropyl
Aminopropyl in base silane is modified to nanoparticle surface；
(A13) heterocyclic pesticide molecule is added in, is had strongly between the aminopropyl of electron rich and the heterocyclic pesticide molecule of electron deficient
Electric charge transfer acts on and forms relatively stable APTS- heterocyclic pesticide molecular complexes；
(A14) it is crosslinking agent using ethylene glycol dimethacrylate, passes through APTS- heterocyclic pesticide molecules after heating polymerization
Compound cures；
(A15) heterocyclic pesticide template molecule is gone by extraction, acidolysis or chemical reaction, obtains that there is heterocyclic pesticide molecular imprinting
Nano artificial antibody；
If the pesticide molecule is organo-chlorine pesticide molecule, step A synthesizes nano artificial antibody as follows：
(A21) nano-particle with hydroxyl is selected as substrate；
(A22) using the hydroxyl on aminopropyl triethoxysilane and nano-particle occur alcoholysis reaction and by three ethoxy of aminopropyl
Aminopropyl in base silane is modified to nanoparticle surface；
(A23) acetate buffer is added in, by aldehyde group modified to nanoparticle surface；
(A24) 2,4- dichlorphenoxyacetic acid organo-chlorine pesticides are added in, APTS- organo-chlorine pesticide molecules are obtained by electric charge transfer and are answered
Close object；
(A25) it is crosslinking agent using ethylene glycol dimethacrylate, is divided by APTS- organo-chlorine pesticides after heating polymerization
Sub- compound curing；
(A26) organo-chlorine pesticide template molecule is gone by extraction, acidolysis or chemical reaction, obtains printing with organo-chlorine pesticide molecule
The nano artificial antibody of note；
In the step B, Nanometer core shell particles are obtained as follows：
(B1) it is coupled using the active group isothiocyanic acid on the amino and fluorescein molecule on aminopropyl triethoxysilane anti-
Should, form the new FITC-APTS function precursors with illuminophore；
(B2) by the polymerisation of FITC-APTS functions precursor and the pesticide molecule marking come directly obtain have concurrently fluorescence labelling with
The Nanometer core shell particles of the pesticide molecule marking；
In the step B, by amino of the nano artificial antibody material micropore inner surface with part with containing active different sulphur cyanogen
The fluorescent molecular reaction of base obtains Nanometer core shell particles after carrying out fluorescence labelling to synthetic nano artificial antibody；
It is characterized in that：In the step C, assembled as follows：
(C1) carrying out hydrophilic treated to optical fiber inner surface by the concentrated sulfuric acid and hydrogen peroxide makes its surface contain more hydroxyl；
(C2) optical fiber inner surface amination is made by aminopropyl triethoxysilane；
(C3) hollow optical fiber inner surface is carried out using the glyoxal of both ends activity aldehyde group modified；
(C4) glyoxal being not bound with fully is washed；
(C5) add in Nanometer core shell particles, amino and the aldehyde radical that glyoxal suspends of Nanometer core shell particles surface residual be mutually bonded from
And Nanometer core shell particles are assembled into hollow optical fiber inner surface, sensor is made.
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| CN110044867B (en) * | 2019-04-08 | 2021-09-21 | 华南理工大学 | In-situ collection and detection device and method for pesticide residues on surfaces of fruits |
| CN112834755B (en) * | 2020-12-31 | 2023-11-17 | 杭州师范大学 | Immune type biosensor detection device based on hollow fiber membrane |
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