CN108344713A - Photonic crystal sensor material and its preparation method and application - Google Patents
Photonic crystal sensor material and its preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of photonic crystal sensor material and its preparation method and application, which includes：In the presence of the first organic solvent and ammonium hydroxide, reaction is hydrolyzed in orthosilicic acid tetraethyl ester, removes first organic solvent and remained ammonia, centrifuges Sieving and casing, silicon ball is made；In the presence of the first organic solvent, silicon ball is mixed with 3 aminopropyl triethoxysilanes, after ultrasound, nitrogen charging deoxygenation, be stirred reaction, amination silicon ball is made；The aqueous solution of amination silicon ball and nano metal solution are subjected to haptoreaction, obtain the amination silicon ball of modified nano gold metal particles；The amination silicon ball of modified nano gold metal particles is subjected to heap base, photonic crystal is made；The photonic crystal is combined with recognition component, the photonic crystal sensor material is made.The photonic crystal sensor material of the present invention detects material as Atrazine, easy to operate when detection, is not necessarily to any pre-treatment, and detection sensitivity height, detection range are wide.
Description
Technical field
The invention belongs to field of pesticide detection, more particularly, to a kind of photonic crystal sensor material and preparation method thereof
And application.
Background technology
Photonic crystal (PC) is to carry out the dielectric material of differing dielectric constant according to certain cycle sequences in space
The orderly periodic structure material with optical wavelength magnitude is formed after arrangement.When light is propagated in the photonic crystal, it may occur that Bradley
Lattice diffraction, diffraction wavelength follow following law：M λ=2ndsin θ, exactly this diffraction make photonic crystal have unique structure
Color.If the lattice parameter of photonic crystal changes, the change of diffraction wavelength can be caused, therefore, photonic crystal is as a kind of
No reagent, unmarked quick detection may be implemented in sensing material.
It realizes the specific detection to object, needs to modify recognition component on photonic, currently, photonic crystal
Common recognition component is some special group (such as phenyl boric acid), molecularly imprinted polymer or aptamers.Song et al. is with third
Olefin(e) acid is monomer, and tetracycline is target, is prepared for counter opal molecular imprinting photonic crystal polymer, realizes to tetracycline
Hypersensitive colorimetric detection.With the increase of tetracycline concentration, the gradual red shift of diffraction wavelength of photonic crystal, schemochrome is also accordingly sent out
Changing.Aptamers polymerize on photonic by Gu et al., are prepared for photonic crystal microcapsules, are used for the detection of mercury ion.
With the increase of ion concentration of mercury, the crosslinking of mercury ion and aptamers causes the contraction of photonic crystal microcapsules, spacing of lattice to become
It is small, it is final that diffraction maximum blue shift occurs, realize the rapid sensitive detection to mercury ion.In addition, also develop can be right by researcher
Na+、K+、Pb2+, bisphenol-A, chloramphenicol, the generations response such as glucose photonic crystal.
But the preparation method of these photonic crystals is all very complicated, particularly with object (such as aflatoxin having
B1, large biological molecule etc.) for, it is difficult to prepare molecular imprinting photonic crystal polymer or imprinting efficiency is too low, causing cannot
Obtain effective response signal；And reach aptamers polymerization to form crosslinked purpose on photonic, then it needs a large amount of
Aptamers, aptamers fancy price limit the further research and application of the photonic crystal.It is a kind of new therefore, it is necessary to develop
Type, convenient for modifying the photon crystal material of various recognition components (aptamers, antibody, receptor etc.).
Invention content
The purpose of the present invention is overcoming the deficiencies of existing technologies, it is brilliant to provide a kind of photon convenient for modifying various recognition components
Body sensing material so that the preparation method of the photonic crystal sensor material is simple, prepared by taking aptamers make recognition component as an example
Photonic crystal sensor material can detect Atrazine, and detect easy to operate, detection sensitivity is high.
To achieve the goals above, the first aspect of the present invention provides a kind of preparation method of photonic crystal sensor material,
The preparation method includes：
(1) in the presence of the first organic solvent and ammonium hydroxide, orthosilicic acid tetraethyl ester is hydrolyzed reaction, described in removal
First organic solvent and remained ammonia centrifuge Sieving and casing, and silicon ball is made；
(2) in the presence of the first organic solvent, the silicon ball is mixed with 3- aminopropyl triethoxysilanes, ultrasound,
After nitrogen charging deoxygenation, it is stirred reaction, amination silicon ball is made；
(3) aqueous solution of amination silicon ball and nano metal solution are subjected to haptoreaction, obtain modified nano gold category
The amination silicon ball of grain；
(4) the amination silicon ball of the modified nano gold metal particles is subjected to heap base, photonic crystal is made；
(5) photonic crystal is combined with recognition component, the photonic crystal sensor material is made.
The second aspect of the present invention provides a kind of photonic crystal sensor material prepared by above-mentioned preparation method.
The third aspect of the present invention provides a kind of above-mentioned photonic crystal sensor material answering as Atrazine detection material
With.
Technical scheme of the present invention has the following advantages that：
1, the present invention connects nano-metal particle, then by modifying upper amino in monodisperse silicon ball surface by amino
The silicon ball heap for having modified nano metal is built into opal photonic crystal, is connected to Atrazine aptamers finally by sulfydryl
The surface of nano-metal particle, to obtain have green gloss, modified the photonic crystal sensor of Atrazine aptamers
Material；Preparation method is simple, and the dosage of aptamers is also few, and cost is greatly saved；In addition, having modified the egg of nanogold
White stone photonic crystal can also modify the large biological molecules such as antibody, receptor, further expand the application of photonic crystal sensor material
Range.
2, the present invention improves diffraction intensity signal, and then be conducive to improve by modified nano gold category on photonic
Detection sensitivity.
3, photonic crystal sensor material of the invention detects material as Atrazine, easy to operate when detection, without times
What pre-treatment, and detection sensitivity is high, and detection range is wide.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Description of the drawings
Exemplary embodiment of the invention is described in more detail in conjunction with the accompanying drawings, it is of the invention above-mentioned and its
Its purpose, feature and advantage will be apparent.
Fig. 1 shows the photonic crystal diffracted signal comparison diagram of the modified nano gold and unmodified nanogold of the present invention.
Specific implementation mode
The preferred embodiment of the present invention is described in more detail below.Although the following describe the preferred implementations of the present invention
Mode, however, it is to be appreciated that may be realized in various forms the present invention without should be limited by embodiments set forth herein.Phase
Instead, these embodiments are provided so that the present invention is more thorough and complete, and can be by the scope of the present invention completely
It is communicated to those skilled in the art.
The first aspect of the present invention provides a kind of preparation method of photonic crystal sensor material, which includes：
(1) in the presence of the first organic solvent and ammonium hydroxide, orthosilicic acid tetraethyl ester is hydrolyzed reaction, described in removal
First organic solvent and remained ammonia centrifuge Sieving and casing, and silicon ball is made；
(2) in the presence of the first organic solvent, the silicon ball is mixed with 3- aminopropyl triethoxysilanes, ultrasound,
After nitrogen charging deoxygenation, it is stirred reaction, amination silicon ball is made；
(3) aqueous solution of amination silicon ball and nano metal solution are subjected to haptoreaction, obtain modified nano gold category
The amination silicon ball of grain；
(4) the amination silicon ball of the modified nano gold metal particles is subjected to heap base, photonic crystal is made；
(5) photonic crystal is combined with recognition component, the photonic crystal sensor material is made.
In the present invention, first organic solvent is preferably absolute ethyl alcohol.
According to the present invention, in step (5), the recognition component can be aptamers, antibody or receptor；When identification member
When part is aptamers, one end of the recognition component is modified with sulfydryl, and the photonic crystal and one end are modified with to the knowledge of sulfydryl
Other element is combined by haptoreaction, and the photonic crystal sensor material is made.
Preferably, when the recognition component is antibody or receptor, by the photonic crystal and recognition component
It is combined by electrostatic adsorption, the photonic crystal sensor material is made.
The present invention modifies upper amino in monodisperse silicon ball surface, and nano-metal particle is connected by amino, then will modification
The silicon ball heap of nano metal is built into opal photonic crystal, and after its drying, buffering containing Atrazine aptamers is added dropwise
One end of solution, aptamers is modified with sulfydryl, and then Atrazine aptamers are connected to the table of nano-metal particle by sulfydryl
Face, to obtain photonic crystal sensor material that there is green gloss, having modified Atrazine aptamers.Simply prepared
Journey, you can detection recognition component is carried on photon crystal micro-ball, and the dosage of aptamers is also few, is greatly saved into
This.In addition, the large biological molecules such as antibody, receptor can also be modified by having modified the opal photonic crystal of nano metal, further open up
The application range of photonic crystal sensor material is opened up.
In accordance with the present invention it is preferred that the nano metal solution is nano-Au solution or Nano silver solution.
Preferably, the preparation method of the nano-Au solution is：By tetramethylol chloride solution and hydroxide
Sodium solution is dispersed in water, and gold chloride is then added, and carries out haptoreaction, and nano-Au solution is made.Wherein, the tetra methylol
The volume ratio of chlorination phosphorus solution and gold chloride is 0.002-0.008:1.
As shown in Figure 1, the photonic crystal of modification gold, the apparent photonic crystal than nanogold is not decorated of diffraction intensity signal
Strong very much (peak shape is more preferable, the high 500a.u. of peak intensity), it follows that modified nano gold is conducive to improve detection on photonic
Sensitivity.
In accordance with the present invention it is preferred that in step (1), the volume ratio of the orthosilicic acid tetraethyl ester and ammonium hydroxide is 0.6-
1.0：1, the catalytic temperature is 20-40 DEG C, reaction time 6-12h.
In accordance with the present invention it is preferred that in step (2), the silicon ball and the volume ratio of 3- aminopropyl triethoxysilanes are
2-10：1, the catalytic temperature is 60-80 DEG C, reaction time 1-10h, preferably 4-8h.
In accordance with the present invention it is preferred that in step (3), the volume ratio of the amination silicon ball and nano metal solution is
0.5-2：1, the catalytic temperature is 20-28 DEG C, reaction time 1-10h, preferably 4-8h.
In accordance with the present invention it is preferred that step (4) includes：By by the mixed liquor of strong acid and strong oxidizer, treated carries
Glass slide cleaning is clean, is placed in vertical exhibition cylinder, is dried up with nitrogen；Then by the amination silicon ball of the modified nano gold metal particles
It pours into the vertical exhibition cylinder, is put into 30-50 DEG C of baking oven and dries, photonic crystal is made.
In accordance with the present invention it is preferred that when the recognition component is aptamers, the photonic crystal is modified with one end
The recognition component of sulfydryl is combined by haptoreaction, and the photonic crystal sensor material is made；The haptoreaction is molten in buffering
It is carried out in the presence of liquid, the buffer solution is phosphate buffer；The catalytic temperature is 20-30 DEG C, the reaction time
Humidity for 10-15h, reaction is 75-85%.
In the present invention, the pH value of the phosphate buffer is preferably 7-8.
In the present invention, photonic crystal is one block of solid material, and photonic crystal and one end are modified with the recognition component of sulfydryl
Haptoreaction is that the solution of the recognition component by one end being modified with sulfydryl is added drop-wise on photonic crystal to realize；This field
Technical staff can determine the dosage of the two as needed.
The second aspect of the present invention provides photonic crystal sensor material prepared by above-mentioned preparation method.
The third aspect of the present invention provides the application that above-mentioned photonic crystal sensor material detects material as Atrazine.
The photonic crystal sensor material of the present invention is immersed in PBS buffer systems and stablizes 30min, by photonic crystal sensor
Material is placed under probe, records initial spike.In order to obtain the optimum reaction condition of aptamers and object, to the reactant
The pH of system is optimized, and Aunar, which is added, by low concentration to high concentration successively under the conditions of pH is 6.6,7.0,7.4,7.8 and 8.0 draws
Tianjin standard solution (methanol：Water=1：4, volume ratio), observe response condition.By optimization, the buffer body that final choice pH is 7.4
It is the preferred testing conditions as the present invention.
The Atrazine standard solution (5 μ g/ml) of maximum concentration is added to the photonic crystal sensor material of the present invention
In PBS buffer systems (pH 7.4), per 1min recording responses signals, after as a result showing 30min, signal reaches stable.
In the PBS buffer systems that pH is 7.4, successively by low concentration to high concentration detection Atrazine (0.1pg/ml-5 μ
G/ml), peak change is recorded, the detection mark song range of linearity for obtaining the photonic crystal sensor material of the present invention is 0.05-
100ng/mL；Lowest detection is limited to 0.5pg/mL.
The photonic crystal sensor material of the present invention is not necessarily to any pre-treatment, directly for surface water such as actual sample lake water
Detection architecture is added, 30min can get stabilization signal, easy to operate, and response is rapid；The response signal of acquisition passes through mark song
The content of Atrazine in surface water can be conversed.
It further illustrates the present invention by the following examples：
Embodiment 1
(1) 150mL absolute ethyl alcohols and 9mL ammonium hydroxide mixings are added in the drying flask of washes clean, adds 7.2mL originals
Tetraethyl silicate (TEOS) is vigorously stirred at 30 DEG C, rotating speed 600rpm, is reacted 9 hours；After reaction by remained ammonia and
Absolute ethyl alcohol removes (rotating speed 4000rpm) by the method for centrifugation, is then dispersed in absolute ethyl alcohol again, is sieved by centrifuging
Grain size (800rpm takes supernatant, 1500rpm to take precipitation), is finally dispersed in 10mL absolute ethyl alcohols by colloidal solid obtained (silicon ball)
Middle preservation；
(2) it takes the silicon ball 1mL of synthesis and is diluted to 10mL with absolute ethyl alcohol, place it in the flask of 50mL, be added 200
μ L3- aminopropyl triethoxysilanes (APTES) and ultrasound 5min, then nitrogen charging deoxygenation 30min, finally machine under the conditions of 70 DEG C
Tool stirs 6 hours, is washed 3 times with ethyl alcohol after the completion of reaction, obtains amination silicon ball, and be resuspended in absolute ethyl alcohol；
(3) sodium hydroxide for the tetramethylol chloride (THPC) and 0.25 μ L2mol/L for being 80% by 12 μ L mass concentrations
It is added in 45mL water, is vigorously stirred 5min, is then quickly added into the gold chloride of 2mL1%, solution colour becomes dark-brown, is protected from light
It is stirred overnight, obtains nano-Au solution；Amination silicon ball is dispersed in again in 10mL water, the nanometer of the above-mentioned acquisitions of 10mL is added
Gold solution mixes ultrasound 15min, is then stirred at room temperature 6 hours, centrifuge washing 5 times after the completion of reaction, obtains modification nanometer
The amination silicon ball of metallic particles is finally resuspended in water so that the later stage uses；
(4) H will be soaked in2SO4：H2O2Volume ratio be 7:It is after 3 mixed liquor and clean with water and washes of absolute alcohol
Glass slide is put into the vertical exhibition cylinder of washes clean, is dried up with nitrogen, and the amination silicon ball of 10mL modified nano gold particles is fallen
Enter to open up in cylinder, be put in 40 DEG C of baking oven and dry, photonic crystal is made；
(5) the aptamers 13000rpm that one end of 200 μ L is modified with to sulfydryl centrifuges 1min, and it is slow that 130 μ L phosphate are added
Fliud flushing (PBS pH=7.4) is diluted to 10mmol/L, and the photonic crystal built is placed in glass culture dish, will be above-mentioned suitable
Ligand solution dropwise addition is positioned in photon crystal surface, and by culture dish in climatic chamber, 25 DEG C of temperature, humidity 80%, instead
It answers 12 hours, photonic crystal sensor material is made.
The photonic crystal sensor material is immersed in the PBS buffer solutions of pH=7.4 and stablizes 30min, successively from low
To the high Atrazine standard solution that various concentration is added, i.e. a concentration of 0.1pg/ml-5 μ g/ml of Atrazine standard solution,
By observing the variation of photonic crystal diffraction peak intensity, it is 0.05-100ng/mL to obtain the detection mark song range of linearity；Minimum detection limit
For 0.5pg/mL.
The embodiment of the present invention is described above, above description is exemplary, and non-exclusive, and also not
It is limited to disclosed embodiment.Without departing from the scope and spirit of embodiment described, for the art
Those of ordinary skill for many modifications and changes will be apparent from.
Claims (10)
1. a kind of preparation method of photonic crystal sensor material, which is characterized in that the preparation method includes：
(1) in the presence of the first organic solvent and ammonium hydroxide, reaction, removal described first is hydrolyzed in orthosilicic acid tetraethyl ester
Organic solvent and remained ammonia centrifuge Sieving and casing, and silicon ball is made；
(2) in the presence of the first organic solvent, the silicon ball is mixed with 3- aminopropyl triethoxysilanes, ultrasound, nitrogen charging
After deoxygenation, it is stirred reaction, amination silicon ball is made；
(3) aqueous solution of amination silicon ball and nano metal solution are subjected to haptoreaction, obtain modified nano gold metal particles
Amination silicon ball；
(4) the amination silicon ball of the modified nano gold metal particles is subjected to heap base, photonic crystal is made；
(5) photonic crystal is combined with recognition component, the photonic crystal sensor material is made.
2. preparation method according to claim 1, wherein in step (5), the recognition component be aptamers, antibody or
Receptor；When the recognition component is aptamers, one end of the recognition component is modified with sulfydryl.
3. preparation method according to claim 1, wherein the nano metal solution is nano-Au solution or nano silver
Solution.
4. preparation method according to claim 1, wherein in step (1), the body of the orthosilicic acid tetraethyl ester and ammonium hydroxide
Product is than being 0.6-1.0：1, the catalytic temperature is 20-40 DEG C, reaction time 6-12h.
5. preparation method according to claim 1, wherein in step (2), the silicon ball and 3- aminopropyl-triethoxy silicon
The volume ratio of alkane is 2-10：1, the catalytic temperature is 60-80 DEG C, reaction time 1-10h.
6. preparation method according to claim 1, wherein in step (3), the amination silicon ball and nano metal solution
Volume ratio be 0.5-2：1, the catalytic temperature is 20-28 DEG C, reaction time 1-10h.
7. preparation method according to claim 1, wherein step (4) includes：It will be by the mixing of strong acid and strong oxidizer
Treated that glass slide cleans up for liquid, is placed in vertical exhibition cylinder, is dried up with nitrogen；Then by the modified nano gold metal particles
Amination silicon ball pour into the vertical exhibition cylinder, be put into 30-50 DEG C of baking oven and dry, be made photonic crystal.
8. preparation method according to claim 2, wherein when the recognition component is aptamers, by photon crystalline substance
The recognition component that body is modified with sulfydryl with one end is combined by haptoreaction, and the photonic crystal sensor material is made；It is described to connect
It touches reaction to carry out in the presence of buffer solution, the buffer solution is phosphate buffer；The catalytic temperature is 20-
30 DEG C, reaction time 10-15h, the humidity of reaction is 75-85%.
9. photonic crystal sensor material prepared by the preparation method according to any one of claim 1-8.
10. the photonic crystal sensor material described in claim 9 detects the application of material as Atrazine.
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| CN112198121A (en) * | 2020-09-07 | 2021-01-08 | 军事科学院军事医学研究院环境医学与作业医学研究所 | Photonic crystal sensing material for SEB (styrene-ethylene-butadiene-styrene) ultrasensitive detection, preparation method thereof and method for detecting SEB ultrasensitively |
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| CN110967110A (en) * | 2019-11-15 | 2020-04-07 | 西安海的电子科技有限公司 | Preparation method of photosensitive sensor material |
| CN110967110B (en) * | 2019-11-15 | 2021-12-28 | 深圳市全创世纪实业有限公司 | Preparation method of photosensitive sensor material |
| CN112198121A (en) * | 2020-09-07 | 2021-01-08 | 军事科学院军事医学研究院环境医学与作业医学研究所 | Photonic crystal sensing material for SEB (styrene-ethylene-butadiene-styrene) ultrasensitive detection, preparation method thereof and method for detecting SEB ultrasensitively |
| CN113189025A (en) * | 2021-03-05 | 2021-07-30 | 军事科学院军事医学研究院环境医学与作业医学研究所 | Photonic crystal sensing material for quickly detecting ricin in ultrasensitive unmarked manner and preparation method and application thereof |
| CN113189025B (en) * | 2021-03-05 | 2023-01-06 | 军事科学院军事医学研究院环境医学与作业医学研究所 | Photonic crystal sensing material for quickly detecting ricin in ultrasensitive unmarked manner and preparation method and application thereof |
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