CN111978467B - Application of one-dimensional photonic crystal sensor film - Google Patents
Application of one-dimensional photonic crystal sensor film Download PDFInfo
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- CN111978467B CN111978467B CN202010757452.XA CN202010757452A CN111978467B CN 111978467 B CN111978467 B CN 111978467B CN 202010757452 A CN202010757452 A CN 202010757452A CN 111978467 B CN111978467 B CN 111978467B
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- 239000004038 photonic crystal Substances 0.000 title claims abstract description 26
- 229960002715 nicotine Drugs 0.000 claims abstract description 32
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 claims abstract description 31
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000012528 membrane Substances 0.000 claims abstract description 20
- 239000002243 precursor Substances 0.000 claims abstract description 15
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 9
- 238000010828 elution Methods 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 6
- 229920006254 polymer film Polymers 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 2
- 239000003431 cross linking reagent Substances 0.000 claims description 2
- 239000003480 eluent Substances 0.000 claims description 2
- 239000000178 monomer Substances 0.000 claims description 2
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 230000000977 initiatory effect Effects 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000001228 spectrum Methods 0.000 abstract description 11
- 238000001514 detection method Methods 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 3
- 230000003993 interaction Effects 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 238000002310 reflectometry Methods 0.000 description 4
- 230000003595 spectral effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000033310 detection of chemical stimulus Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000010076 replication Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000025508 response to water Effects 0.000 description 1
- 230000005586 smoking cessation Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/26—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a solid phase from a macromolecular composition or article, e.g. leaching out
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- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
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- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/47—Scattering, i.e. diffuse reflection
- G01N21/4738—Diffuse reflection, e.g. also for testing fluids, fibrous materials
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- 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
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- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/24—Homopolymers or copolymers of amides or imides
- C08J2333/26—Homopolymers or copolymers of acrylamide or methacrylamide
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Abstract
The invention relates to an application of a one-dimensional photonic crystal sensor film, belonging to the technical field of photonic crystals and molecular imprinting. The main technical scheme is as follows: covering the precursor liquid with a photonic crystal template, placing the precursor liquid under an ultraviolet lamp to initiate polymerization, removing the membrane after complete polymerization, and eluting to obtain the molecularly imprinted membrane with the one-dimensional photonic crystal structure. The micro detection of nicotine can be realized according to the reflection spectrum change of the molecularly imprinted membrane prepared by the one-dimensional photonic crystal sensor membrane, the detection is carried out according to the reflection spectrum change of the interaction of chemical substances with different concentrations and the molecularly imprinted membrane, the complicated steps of the traditional detection method can be avoided, the detected reflection spectrum change is obvious, and the sensitivity is higher, so that the observation is convenient.
Description
Technical Field
The invention relates to the technical field of photonic crystals and molecular imprinting, in particular to application of a one-dimensional photonic crystal sensor film.
Background
The molecular imprinting technology is a preparation technology for obtaining a polymer which is completely matched with a specific template molecule on a spatial structure and a binding site, and is a process for preparing and obtaining a molecule with specific selectivity.
Disclosure of Invention
The invention provides an application of a one-dimensional photonic crystal sensor film for preparing a molecularly imprinted film, which comprises the following specific steps: covering the precursor liquid with a photonic crystal template, placing the precursor liquid under an ultraviolet lamp to initiate polymerization, removing the membrane after complete polymerization, and eluting to obtain the molecularly imprinted membrane with the one-dimensional photonic crystal structure.
The one-dimensional photonic crystal sensor film with the span of 761nm, the height of 75nm and the step pitch of 350nm is adopted, the photonic crystal and the molecular imprinting technology are combined, and the change of the reflection spectrum intensity of the sensor film is measured by an optical spectrometer according to the different effects of nicotine with different concentrations on the molecular imprinting polymer film, so that the nicotine content can be measured.
The detection principle is as follows: when white incident light is irradiated on the sensor surface, the wavelength of the reflected light conforms to the grating equation: m λ ═ d (sin θ) 1 +θ D ) Where m is the number of diffraction orders, λ is the wavelength of diffracted light, θ 1 Is the light source incident angle; theta D Is the angle of reflection; d is the grating period.
When sample molecules enter the holes on the nicotine molecular imprinting film, nicotine molecules are combined in the holes, the combination can cause the structure of the nicotine molecular imprinting film to be slightly changed, the surface morphology of the molecular imprinting film, namely the height on the film, is changed, the changes can cause the reflectivity of the photonic crystal reflecting film to be changed macroscopically, and the change of the reflectivity is in direct proportion to the concentration logarithm of the nicotine sample molecules, so that the nicotine concentration can be measured according to the change of a reflection spectrum. This detection is specific because the molecularly imprinted membrane is unique to the nicotine molecule.
The invention has the following beneficial effects:
(1) the invention uses a template replication method, utilizes ultraviolet light to initiate polymerization to prepare the photonic crystal molecular imprinting sensor, has simple preparation method, and can greatly shorten the preparation time;
(2) the micro detection of chemical substances such as nicotine and the like can be realized by combining the molecular imprinting technology;
(3) according to the change of the reflection spectrum of the interaction between the chemical substances with different concentrations and the molecularly imprinted membrane, the complicated steps of the traditional detection method can be avoided, the detected reflection spectrum has obvious change, the sensitivity is higher, and the observation is convenient, so that the rapid visual detection of the chemical substances such as nicotine and the like can be realized.
Drawings
FIG. 1 is a scanning electron microscope image of a one-dimensional photonic crystal template;
FIG. 2 is a comparison of the spectra of a molecularly imprinted membrane before and after elution and a non-molecularly imprinted membrane (NMIP); wherein: a. NMIP, b, after elution, c, before elution.
FIG. 3 is a graph of the response of a molecularly imprinted membrane to different concentrations of nicotine;
wherein: a. water, b, 10 -9 mol/L，c、10 -8 mol/L，d、10 -7 mol/L，e、10 -6 mol/L，f、10 -5 mol/L。
Figure 4 is a graph of nicotine at different concentrations plotted against the corresponding spectral reflectance.
Detailed Description
The technical solution of the present invention is further described below with reference to specific examples, but the present invention is not limited to the contents of the examples in any way. In the examples, unless otherwise specified, the test methods are conventional methods; unless otherwise specified, the reagents and biomaterials are commercially available.
The application method provided by the invention can be used for detecting nicotine molecules.
EXAMPLE 1 preparation of precursor solution
(1) Template molecules nicotine (1.00mmol), functional monomers acrylamide (30.96mmol) and methacrylic acid (7.29mmol) and cross-linking agent N, N' -methylenebisacrylamide (0.55mmol) were added to a round bottom flask containing 2.4mL of methanol and mixed, stirred overnight for 12 hours at 25 ℃;
(2) adding photoinitiator UV 1173(0.081mmol) into the solution, stirring uniformly for 30min, and deoxidizing with nitrogen for 5min to obtain the polymer precursor solution.
Example 2 preparation of Polymer films
(1) Taking a clean glass sheet, dropwise adding 250 mu L of the prepared precursor liquid on the glass sheet, and then slowly covering a one-dimensional photonic crystal template which is 20mm multiplied by 20mm, has a span of 761nm and a height of 75nm on the solution along one side of the precursor liquid, wherein no air bubbles can appear, and the photonic crystal template is shown as an attached drawing 1;
(2) and (3) placing the glass sheet under an ultraviolet lamp to initiate polymerization for 2h, and removing the film after complete polymerization.
Example 3 preparation of a nicotine molecularly imprinted membrane
(1) Preparing a solution of 10mL of methanol and acetic acid (9: 1), placing the one-dimensional photonic crystal polymer film polymerized in the example 2 into the solution, and performing ultrasonic washing;
(2) changing the eluent once every 15min of ultrasonic treatment, changing for 4 times, and carrying out ultrasonic elution for 1h in total;
(3) after the ultrasonic elution is finished, the surface of the molecularly imprinted membrane is washed by a methanol solution to wash off the redundant acetic acid solution, so that the nicotine molecularly imprinted membrane is obtained, and the result is shown in figure 2.
EXAMPLE 4 determination of nicotine
The prepared nicotine molecular imprinting film is taken and respectively placed in nicotine solution with different concentrations for 5min, the film is taken out, and the reflection spectrum is immediately measured by a spectrometer, and the result is shown in figure 3. As can be seen from the figure, the molecularly imprinted membrane has no response to water and gradually reduces the intensity of the reflection peak with the increase of the concentration when responding to nicotine, and when the concentration is reduced to 10 -9 At mol/L, the minimum concentration detectable by the molecularly imprinted membrane is reached. To better understand the concentration versus reflectance, a linear fit was made between the negative logarithm of the nicotine concentration and the corresponding reflectance, and the results are shown in fig. 4. It can be seen from the figure that the negative logarithm of nicotine concentration and its reflectivity show good linear relation, the linear equation is-logC ═ R/4.53-10.22(R is reflectivity at maximum wavelength of reflection spectrum, C-nicotine concentration), and the correlation coefficient is 0.9890. Therefore, the molecularly imprinted membrane can be used for rapidly detecting a lower content nicotine solution.
EXAMPLE 5 determination of Nicotine in samples
And (3) placing the nicotine molecular imprinting film in a treated solution to be tested for smoking cessation sugar for 5min, taking out, and measuring the film reflection spectrum by a spectrometer. Calculating to obtain the nicotine concentration of 3.41 × 10 in the sample according to the linear relation equation of the negative logarithm of the nicotine concentration and the spectral reflectance thereof -6 mol/L。
Claims (1)
1. The application of the one-dimensional photonic crystal sensor film is characterized in that the one-dimensional photonic crystal sensor film is used for preparing a molecularly imprinted film, a photonic crystal template is covered on precursor liquid, the precursor liquid is placed under an ultraviolet lamp to initiate polymerization, the film is removed after the precursor liquid is completely polymerized, and the molecularly imprinted film with the one-dimensional photonic crystal structure is obtained after elution;
the method comprises the following specific steps:
step S1: preparation of precursor solution
(1) 1.00mmol of template molecule nicotine, 30.96mmol of functional monomer acrylamide, 7.29mmol of methacrylic acid and 0.55mmol of cross-linking agent N, N' -methylenebisacrylamide are added into a round-bottom flask containing 2.4mL of methanol for mixing, and the mixture is stirred overnight for 12 hours at 25 ℃;
(2) adding 0.081mmol of photoinitiator UV 1173 into the solution, uniformly stirring for 30min, and deoxidizing for 5min by using nitrogen to obtain polymer precursor solution;
step S2: preparation of Polymer films
(1) Taking a clean glass sheet, dropwise adding 250 mu L of the prepared precursor solution on the glass sheet, and then slowly covering a one-dimensional photonic crystal template with a span of 20mm multiplied by 20mm being 761nm and a height of 75nm on the solution along one side of the precursor solution;
(2) placing the glass sheet under an ultraviolet lamp for initiating polymerization for 2h, and removing the film after complete polymerization;
step S3: preparation of nicotine molecular imprinting film
(1) Preparing a solution of 10mL of methanol and acetic acid =9:1, placing the one-dimensional photonic crystal polymer film polymerized in the step S2 into the solution, and performing ultrasonic washing;
(2) changing the eluent once every 15min of ultrasonic treatment, changing for 4 times, and carrying out ultrasonic elution for 1h in total;
(3) and after ultrasonic elution, washing the surface of the molecularly imprinted membrane by using a methanol solution to wash off redundant acetic acid solution, thus obtaining the nicotine molecularly imprinted membrane.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101088426A (en) * | 2007-07-13 | 2007-12-19 | 湖南中烟工业公司 | Molecular imprinting material for lowering nicotine content in cigarette fume selectively and its application |
| EP2500314A1 (en) * | 2011-03-14 | 2012-09-19 | Nederlandse Organisatie voor toegepast -natuurwetenschappelijk onderzoek TNO | Photonic crystal sensor |
| EP3526782A1 (en) * | 2016-10-13 | 2019-08-21 | DrinkSavvy, Inc. | Colorimetric chemical sensor with enhanced color sensitivity |
| CN109900653B (en) * | 2019-01-25 | 2021-09-07 | 南阳师范学院 | Molecularly imprinted photonic crystal film for rapidly detecting lysozyme and preparation method and application thereof |
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