CN110668442A - Based on Ti3C2TXModified biosensing surface, preparation method and application thereof - Google Patents
Based on Ti3C2TXModified biosensing surface, preparation method and application thereof Download PDFInfo
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- CN110668442A CN110668442A CN201910848983.7A CN201910848983A CN110668442A CN 110668442 A CN110668442 A CN 110668442A CN 201910848983 A CN201910848983 A CN 201910848983A CN 110668442 A CN110668442 A CN 110668442A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 238000001514 detection method Methods 0.000 claims abstract description 22
- 239000000758 substrate Substances 0.000 claims abstract description 14
- 239000004475 Arginine Substances 0.000 claims abstract description 13
- 229910009819 Ti3C2 Inorganic materials 0.000 claims abstract description 13
- ODKSFYDXXFIFQN-UHFFFAOYSA-N arginine Natural products OC(=O)C(N)CCCNC(N)=N ODKSFYDXXFIFQN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 13
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 5
- 150000003624 transition metals Chemical class 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 9
- 238000005530 etching Methods 0.000 claims description 8
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 7
- 239000010931 gold Substances 0.000 claims description 7
- 229910052737 gold Inorganic materials 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 5
- 229910009818 Ti3AlC2 Inorganic materials 0.000 claims description 3
- 230000002378 acidificating effect Effects 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 239000012047 saturated solution Substances 0.000 claims description 3
- 241000446313 Lamella Species 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 125000000637 arginyl group Chemical group N[C@@H](CCCNC(N)=N)C(=O)* 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000725 suspension Substances 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 description 7
- 239000000956 alloy Substances 0.000 description 6
- 150000003384 small molecules Chemical class 0.000 description 4
- 238000000572 ellipsometry Methods 0.000 description 3
- 238000003384 imaging method Methods 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000037007 arousal Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012472 biological sample Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000004634 pharmacological analysis method Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/921—Titanium carbide
-
- 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
- G01N21/21—Polarisation-affecting properties
- G01N21/211—Ellipsometry
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- 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
- G01N21/21—Polarisation-affecting properties
- G01N21/211—Ellipsometry
- G01N2021/212—Arrangement with total internal reflection
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
- Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)
Abstract
The invention belongs to the technical field of biosensor preparation, and particularly relates to a Ti-based biosensor3C2TxModified biosensing surfaces, methods of making and uses thereof. The Ti base3C2TxA modified biosensing surface comprising: sensing substrate and Ti with modified surface3C2Tx(ii) a Wherein T isxIs a surface group O2‑、OH‑、F‑、NH3、NH4+. By adding a transition metal carbide Ti3C2TxThe biological sensing substrate is coated to form a sensing surface which can be used for adsorbing charged small biological molecules, so that the detection capability of the small biological molecules is improved. The method is convenient to operate, and compared with the sensing surface of the traditional total internal reflection biosensor, the detection limit of arginine is improved by 100 times, and the requirement of arginine detection can be metAnd (5) actually detecting the demand.
Description
Technical Field
The invention belongs to the technical field of biosensor preparation, and particularly relates to a Ti-based biosensor3C2TxModified biosensing surfaces, methods of making and uses thereof.
Background
The total internal reflection ellipsometric imaging biosensor is an optical biosensor which can be used for researching the adsorption behavior of biomolecules on a solid phase surface. The method uses changes of optical properties such as spectral absorption, reflection and refractive index caused by adsorption of biomolecules on a solid phase surface as a detection means, and has the advantages of small damage to biological samples and high detection sensitivity. Meanwhile, as the sample for detection can usually avoid complicated pretreatment steps, the total internal reflection ellipsometry imaging biosensor can be used for real-time and high-flux sample detection, and thus has wide application in various fields such as biomedical research, disease diagnosis, pharmacy, food safety, environmental monitoring and the like.
However, with the increasing medical level and arousal of people's health and environmental awareness, people have raised higher requirements on the total internal reflection ellipsometry biosensor in the aspects of early disease detection, pharmacological analysis and trace pollution detection. The existing total internal reflection ellipsometry imaging biosensor has higher detection sensitivity for protein and other biological macromolecules, but has the problems of low adsorption capacity and incapability of carrying out effective analysis on the interaction of biological molecules for amino acid and other biological micromolecules.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
In order to solve the technical problem, the invention provides a Ti-based alloy3C2TxThe modified biosensing surface effectively improves the adsorption capacity of charged biological small molecules on the biosensing surface.
The Ti base3C2TxA modified biosensing surface comprising: sensing substrate and Ti with modified surface3C2Tx(ii) a Wherein, TxIs a surface group O2-、OH-、F-、NH3、NH4+。
By modifying the surface of a conventional sensing substrate with transition metal carbide Ti3C2TxThe adsorption capacity of the biological micromolecules on the sensing surface can be obviously improved, and the detection limit of the biosensor is further improved.
Further, the surface of the sensing substrate is plated with a gold film. Preferably, the gold film has a thickness of 50 nm.
The invention also provides the Ti-based alloy3C2TxA method of preparing a modified biosensing surface comprising:
(1) etching MAX phase Ti by using LiF/HCl mixed solution3AlC2To obtain a transition metal carbide Ti3C2Tx;
(2) Immersing the sensing substrate plated with the gold film into Ti3C2TxIn saturated solution, Ti due to electrostatic effect3C2TxAnd attaching the film on the surface of the sensing substrate to obtain the film.
The step (1) comprises the following specific operation steps:
(1) dissolving LiF in HCl to prepare etching solution;
(2) mixing Ti3AlC2Gradually adding the mixture into etching liquid, and reacting to obtain an acid product;
(3) repeatedly washing the obtained acidic product with deionized water, and centrifuging to obtain dark green Ti3C2TxLamellar suspension; at the moment, the pH value of the system is more than or equal to 6; adding deionized water into the precipitate, shaking by hand, separating the lamella, performing ultrasonic treatment, and centrifuging the obtained solution to obtain the final product.
The invention also provides the Ti-based alloy3C2TxUse of a modified biosensing surface for the detection of small biological molecules. The biological small molecule is arginine.
The invention also provides a potential modulation type total internal reflection biosensor, which comprises the Ti-based biosensor3C2TxA modified biosensing surface.
The invention also provides a method for detecting arginine, which comprises the following steps: detection was performed using the potential-modulated total internal reflection biosensor described above, in which-50 mV was applied to the sensing surface. By applying a specific voltage, the adsorption amount of arginine on the sensing surface can be significantly increased.
The invention has the following beneficial effects:
hair brushObviously utilizing transition metal carbide Ti3C2TxThe biological sensing substrate is coated, and a sensing surface for adsorbing charged biological small molecules is formed by applying a specific surface potential, so that the detection capability of the biological small molecules is improved. The method is convenient to operate, and compared with the sensing surface of the traditional total internal reflection biosensor, the detection limit of arginine is improved by 100 times, and the actual detection requirement can be met.
Drawings
FIG. 1 is a Ti-based alloy as described in example 13C2TXSchematic diagram of the preparation process of the modified biosensing surface.
FIG. 2 is a Ti-based alloy utilizing a Ti base as described in example 23C2TxSchematic diagram of modified biosensing surface for detecting arginine.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
This example provides a Ti-based alloy3C2TXA method of preparing a modified biosensing surface, as shown in figure 1, comprising:
(1)1g LiF is completely dissolved in 20ml 9M HCl to prepare etching solution;
(2) mixing 1g of Ti3AlC2Gradually adding into the etching solution, and reacting at 35 deg.C for 24 hr;
(3) the resulting acidic product was repeatedly rinsed with deionized water and centrifuged at 3500rpm for 5 minutes until stable dark green Ti was obtained3C2TxAnd (4) suspending the sheet layer. At the moment, the pH value of the solution is more than or equal to 6; deionized water was added to the precipitate and shaken by hand for 5 minutes to separate the sheets. After 1 hour of sonication, the resulting solution was centrifuged at 3500rpm for 1 hour to obtain Ti3C2TxSuspending the solution;
(4) immersing the substrate plated with the 50nm gold film into Ti3C2TxSaturated solution, reaction at 4 deg.C for 60 hr, Ti due to electrostatic effect3C2TxWill be attached to the surface of the sensing substrate and modified with Ti3C2TxThe preparation of the biosensing surface of (2) is completed.
Example 2
This example provides a potential-modulated total internal reflection biosensor comprising the Ti-based biosensor obtained in example 13C2TxA modified biosensing surface.
Example 3
The present embodiment provides a method for detecting arginine using the potential-modulated total internal reflection biosensor obtained in embodiment 2, which specifically comprises: during detection, a voltage of-50 mV is applied to the sensing surface so as to increase the adsorption of arginine on the surface.
Through detection, compared with the traditional arginine detection method, the method disclosed in the example 3 can improve the arginine detection limit by 100 times.
The specific detection principle is shown in fig. 2.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. Based on Ti3C2TxA modified biosensing surface, comprising: sensing substrate and Ti with modified surface3C2Tx(ii) a Wherein T isxIs a surface group O2-、OH-、F-、NH3、NH4+。
2. The biosensing surface of claim 1, wherein said sensing substrate is coated with a gold film.
3. The biosensing surface according to claim 1 or 2, wherein the gold film has a thickness of 50 nm.
4. A method of preparing a biosensing surface according to any of claims 1 to 3, comprising:
(1) etching MAX phase Ti by using LiF/HCl mixed solution3AlC2To obtain a transition metal carbide Ti3C2Tx;
(2) Immersing the sensing substrate plated with the gold film into Ti3C2TxIn a saturated solution of (2), Ti due to electrostatic action3C2TxAnd attaching the film on the surface of the sensing substrate to obtain the film.
5. The preparation method according to claim 4, wherein the step (1) is carried out by the following steps:
(1) dissolving LiF in HCl to prepare etching solution;
(2) mixing Ti3AlC2Gradually adding the mixture into etching liquid, and reacting to obtain an acid product;
(3) repeatedly washing the obtained acidic product with deionized water, and centrifuging to obtain dark green Ti3C2TxLamellar suspension; at the moment, the pH value of the system is more than or equal to 6; adding deionized water into the precipitate, shaking by hand, separating the lamella, performing ultrasonic treatment, and centrifuging the obtained solution to obtain the final product.
6. Use of a biosensing surface according to any of claims 1 to 3 for the detection of small biological molecules.
7. The use of claim 6, wherein the small biological molecule is arginine.
8. A potential-modulated total internal reflection biosensor comprising a biosensing surface according to any of claims 1-3.
9. A method for detecting arginine comprising: detection is carried out using a biosensing surface according to any of claims 1 to 3.
10. The method of claim 9, wherein-50 mV is applied to the biosensing surface.
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Cited By (1)
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CN113636555A (en) * | 2021-08-30 | 2021-11-12 | 北京航空航天大学 | Ti3C2TxOxygen vacancy anchoring single-atom material and preparation method and application thereof |
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CN113636555A (en) * | 2021-08-30 | 2021-11-12 | 北京航空航天大学 | Ti3C2TxOxygen vacancy anchoring single-atom material and preparation method and application thereof |
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Application publication date: 20200110 |