CN108693150A - The application of porous sheet carbonitride - Google Patents
The application of porous sheet carbonitride Download PDFInfo
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- CN108693150A CN108693150A CN201710230495.0A CN201710230495A CN108693150A CN 108693150 A CN108693150 A CN 108693150A CN 201710230495 A CN201710230495 A CN 201710230495A CN 108693150 A CN108693150 A CN 108693150A
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- uric acid
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- solution
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- 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
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/645—Specially adapted constructive features of fluorimeters
- G01N21/6456—Spatial resolved fluorescence measurements; Imaging
- G01N21/6458—Fluorescence microscopy
Abstract
A kind of application the invention discloses porous sheet carbonitride as fluorescence probe in detecting micro uric acid.The excellent photoluminescence performance that graphite phase carbon nitride itself has, can send out fluorescence under certain exciting light;By the interlayer structure for having removed carbonitride to graphite phase carbon nitride acid etching, supersound process, simultaneously so that modified porous sheet carbonitride aqueous stability has and is greatly improved, and the introducing of a variety of oxygen-containing groups is conducive to form stable hydrogen bond between probe and detectable substance uric acid, and it can more effective fixed test object.PCN fluorescence probes used in the present invention are prepared simply, environmental friendly, of low cost;Have the characteristics that the response time is fast, the range of linearity is wide, favorable reproducibility, stability are high in for fluorescence detection simultaneously, to the detection of micro metabolin with extensive Research Prospects in future medicine research.
Description
Technical field
The present invention relates to field of nanometer material technology and field of fluorescence, nitrogenizing nano material porous sheet more particularly to a kind of
Carbon detects uric acid concentration in terms of being applied to fluorescence sense.
Background technology
g-C3N4, i.e. the C of graphite-phase3N4, it is five kinds of C3N4In most stable of one kind.About g-C3N4Single layer structure, people
There are mainly two types of different views:One kind thinking single layer g-C3N4With triazine ring (C3N3Ring) it is structural unit;Another kind thinks single
Layer g-C3N4Basic structural unit be 3-s- triazine rings (C6N7Ring).It is calculated by Density functional (DFT), is based on 3-s- triazines
The g-C of ring3N4Structure is than the g-C based on triazine ring3N4Stable structure, it is in recent years, most of to g-C3N4Research all with 3-s-
Triazine ring structure is theoretical model.In nature, so far it has not been found that there are natural g-C3N4Crystal.So g-C3N4
Research dependent on experiment synthesize.Suitable carbon source and nitrogen source react g-C can be obtained under certain condition3N4, common reactant
There are melamine, cyanuric trichloride, cyanamide, dicyanodiamine, urea etc..At present, g-C3N4Primary synthetic methods have:High temperature and pressure
Method, solvent-thermal method, sedimentation, thermal polymerization etc..Thermal polymerization can react item conveniently by other substances are added or change
Part adjusts g-C3N4Structure, to improve g-C3N4Properties, be current g-C3N4Common synthetic method in research.
Graphite phase carbon nitride (g-C at present3N4) application be concentrated mainly on photocatalysis and electrochemical sensing in terms of.As
A kind of visible light-responded semi-conducting polymer photochemical catalyst, g-C3N4With cheap and easy to get, chemical stability is good, nontoxic
And the advantages that suitable energy gap and position of energy band, simultaneously because its quite a high proportion of N content makes g-C3N4It shows
Excellent catalytic performance, thus there are more and more scientific workers to be ground in the performance of electrochemical sensing for carbonitride
Study carefully.However g-C3N4There is also can only absorbing wavelength less than 475nm light, photo-generated carrier it is compound serious the problems such as, need to it
It is modified to improve photo-catalysis capability;In terms of electrochemical sensing, g-C3N4Low electric conductivity limit so that its must be with other
The material progress of high conduction performance is compound to be used in electrochemical sensing.
Invention content
The object of the present invention is to provide a kind of porous sheet carbon nitride materials efficiently to measure uric acid concentration as fluorescence probe
Application.
Realizing the technical solution of the object of the invention is:Porous sheet carbonitride (PCN) detects micro- as fluorescence probe
Measure the application of uric acid.
In the application, compound concentration is the PCN solution of 0.05~0.15mg/ml as fluorescence probe.
In the application, a concentration of 0.05 μM~10 μM of micro uric acid.
Compared with prior art, the present invention its remarkable advantage is:(1) PCN fluorescence probes preparation process is simple, prepares
Journey easy operation control, it is of low cost;(2) PCN material surfaces have the dissolubility of abundant oxygen-containing group raising in aqueous solution,
The active force between detection molecules is enhanced, larger specific surface area provides sufficient reaction compartment for chemical reaction;(3)
PCN fluorescence probes show excellent sensitivity and anti-interference on detection uric acid concentration, and the response time is fast, low detection limit,
It is easy to operation.
Description of the drawings
The detects schematic diagram of PCN fluorescence probes in Fig. 1 Figure of abstract.
PCN probes transmission electron microscope figure in Fig. 2 embodiments one (wherein, A is PCN surface topographies under low amplification factor,
B is PCN surface topographies under high-amplification-factor).
In Fig. 3 embodiments one fluorescent emission figure (figure A) of PCN probe in detecting various concentration uric acid and uric acid concentration with it is glimmering
The linear relationship chart (figure B) of luminous intensity.
In Fig. 4 embodiments two fluorescent emission figure (figure A) of PCN probe in detecting various concentration uric acid and uric acid concentration with it is glimmering
The linear relationship chart (figure B) of luminous intensity.
In Fig. 5 embodiments three fluorescent emission figure (figure A) of PCN probe in detecting various concentration uric acid and uric acid concentration with it is glimmering
The linear relationship chart (figure B) of luminous intensity.
In Fig. 6 example IVs the fluorescent emission figure (figure A) of PCN probe in detecting various concentration uric acid and uric acid concentration with it is glimmering
The linear relationship chart (figure B) of luminous intensity.
In Fig. 7 embodiments five fluorescent emission figure (figure A) of PCN probe in detecting various concentration uric acid and uric acid concentration with it is glimmering
The linear relationship chart (figure B) of luminous intensity.
Specific implementation mode
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.
Embodiment one
(1) preparation of porous sheet carbonitride PCN:It takes 10g urea to be placed in ceramic crucible, crucible tinfoil is coated into shape
It is calcined at semiclosed system and being put into Muffle furnace, 4h is calcined at 550 DEG C;The g-C that will be burnt out3N4Grind into powder juxtaposition
In beaker, then the 10ml concentrated sulfuric acids and 30ml concentrated nitric acids progress acid etching are added into beaker, are sealed beaker system with polyethylene film
Mild ultrasound 12h in standby water bath sonicator instrument;By g-C after acid etching ultrasound3N4Mixed acid solution be diluted to deionized water
200ml filters the solution after dilution using 0.45 μm of miillpore filter and collects filter residue;By ultrasound by filter residue again
It is distributed in the distilled water of 16ml, obtains the porous sheet carbonitride PCN of stable dispersion in water.
(2) preparation of PCN probes:PCN solution is diluted to 0.1mg/ml, takes the 2ml solution and PCN is made in ultrasound 30min
Fluorescence probe.
(3) determination of PCN probes excitation wavelength:PCN is first excited with rough excitation wavelength with reference to pertinent literature, is sent out
Penetrate peak position;It is counter on the basis of the emission peak positions again to sweep PCN, obtain PCN excitation wavelength ranges;Finally to excitation wave in range
Long experiment one by one obtains to inspire the wavelength of most strong emission peak.
(4) uric acid concentration measures in solution:A certain amount of uric acid (0.05~10 μM) is added into PCN probe solutions, and
Its emission spectrum, Strength Changes of the recording solution emission peak after UA is gradually added dropwise are measured at maximum excitation wavelength λ=320nm
(quenching or enhancing).
(5) it establishes the relational expression of solution emission peak variation tendency and UA concentration and calculates minimum detection limit.
As shown in Figure 1, the BCN with stacked structure is stripped into sheet and PCN fluorescence is made in its surface etch pore-forming
Probe.After uric acid is added, uric acid molecule can be with PCN Binding change solution fluorescence intensity.
As shown in Fig. 2, being PCN probe transmission electron microscope figures, as can be seen from the figure PCN has small and thin lamella
Porous structure and hole is evenly distributed, thus the material has big specific surface area.
As shown in figure 3, the uric acid (0.05~10 μM) of various concentration is added separately in the fluorescence probe of 0.1mg/ml, make
The linear of uric acid concentration and fluorescence intensity is measured while obtained to the fluorescent emission intensity of solution with sepectrophotofluorometer
Relationship.As a result show the PCN fluorescence probes to uric acid have good linear relationship, high sensitivity, wide detection range and
Low detection limit.
Embodiment two
(1) the porous sheet carbonitride PCN in embodiment one is made.
(2) preparation of PCN probes:PCN solution is diluted to 0.05mg/ml, takes the 2ml solution and PCN is made in ultrasound 30min
Fluorescence probe.
(3) determination of PCN probes excitation wavelength:PCN is first excited with rough excitation wavelength with reference to pertinent literature, is sent out
Penetrate peak position;It is counter on the basis of the emission peak positions again to sweep PCN, obtain PCN excitation wavelength ranges;Finally to excitation wave in range
Long experiment one by one obtains to inspire the wavelength of most strong emission peak.
(4) uric acid concentration measures in solution:It is added a certain amount of uric acid (0.5~10 μM) into PCN probe solutions, and
Its emission spectrum, Strength Changes of the recording solution emission peak after UA is gradually added dropwise are measured at maximum excitation wavelength λ=320nm
(quenching or enhancing).
(5) it establishes the relational expression of solution emission peak variation tendency and UA concentration and calculates minimum detection limit.
As shown in figure 4, the uric acid (0.05~10 μM) of various concentration is added separately in the fluorescence probe of 0.15mg/ml,
Uric acid concentration and the line of fluorescence intensity are measured while obtained to the fluorescent emission intensity of solution using sepectrophotofluorometer
Sexual intercourse.
Embodiment three
(1) the porous sheet carbonitride PCN in embodiment one is made.
(2) preparation of PCN probes:PCN solution is diluted to 0.15mg/ml, takes the 2ml solution and PCN is made in ultrasound 30min
Fluorescence probe.
(3) determination of PCN probes excitation wavelength:PCN is first excited with rough excitation wavelength with reference to pertinent literature, is sent out
Penetrate peak position;It is counter on the basis of the emission peak positions again to sweep PCN, obtain PCN excitation wavelength ranges;Finally to excitation wave in range
Long experiment one by one obtains to inspire the wavelength of most strong emission peak.
(4) uric acid concentration measures in solution:A certain amount of uric acid (0.05~10 μM) is added into PCN probe solutions, and
Its emission spectrum is measured at excitation wavelength lambda=320nm, Strength Changes of the recording solution emission peak after UA is gradually added dropwise are (sudden
It goes out or enhances).
(5) it establishes the relational expression of solution emission peak variation tendency and UA concentration and calculates minimum detection limit.
As shown in figure 5, the uric acid (0.05~10 μM) of various concentration is added separately in the fluorescence probe of 0.05mg/ml,
Uric acid concentration and the line of fluorescence intensity are measured while obtained to the fluorescent emission intensity of solution using sepectrophotofluorometer
Sexual intercourse.
Example IV
(1) the porous sheet carbonitride PCN in embodiment one is made.
(2) preparation of PCN probes:PCN solution is diluted to 0.10mg/ml, takes the 2ml solution and PCN is made in ultrasound 30min
Fluorescence probe.
(3) determination of PCN probes excitation wavelength:PCN is first excited with rough excitation wavelength with reference to pertinent literature, is sent out
Penetrate peak position;It is counter on the basis of the emission peak positions again to sweep PCN, obtain PCN excitation wavelength ranges;Finally to excitation wave in range
Long experiment one by one obtains to inspire the wavelength of most strong emission peak.
(4) uric acid concentration measures in solution:A certain amount of uric acid (0.01~50 μM) is added into PCN probe solutions, and
Its emission spectrum is measured at excitation wavelength lambda=320nm, Strength Changes of the recording solution emission peak after UA is gradually added dropwise are (sudden
It goes out or enhances).
(5) it establishes the relational expression of solution emission peak variation tendency and UA concentration and calculates minimum detection limit.
As shown in fig. 6, the uric acid (0.01~50 μM) of various concentration is added separately in the fluorescence probe of 0.1mg/ml, make
The linear of uric acid concentration and fluorescence intensity is measured while obtained to the fluorescent emission intensity of solution with sepectrophotofluorometer
Relationship.
Embodiment five
(1) the porous sheet carbonitride PCN in embodiment one is made.
(2) preparation of PCN probes:PCN solution is diluted to 0.10mg/ml, takes the 2ml solution and PCN is made in ultrasound 30min
Fluorescence probe.
(3) determination of PCN probes excitation wavelength:PCN is first excited with rough excitation wavelength with reference to pertinent literature, is sent out
Penetrate peak position;It is counter on the basis of the emission peak positions again to sweep PCN, obtain PCN excitation wavelength ranges;Finally to excitation wave in range
Long experiment one by one obtains to inspire the wavelength of most strong emission peak.
(4) uric acid concentration measures in solution:A certain amount of uric acid (0.01~0.5 μM) is added into PCN probe solutions, and
Its emission spectrum is measured at excitation wavelength lambda=320nm, Strength Changes of the recording solution emission peak after UA is gradually added dropwise are (sudden
It goes out or enhances).
(5) it establishes the relational expression of solution emission peak variation tendency and UA concentration and calculates minimum detection limit.
As shown in fig. 7, the uric acid (0.01~0.5 μM) of various concentration is added separately in the fluorescence probe of 0.1mg/ml,
Uric acid concentration and the line of fluorescence intensity are measured while obtained to the fluorescent emission intensity of solution using sepectrophotofluorometer
Sexual intercourse.
Claims (3)
1. application of the porous sheet carbonitride as fluorescence probe in detecting micro uric acid.
2. application as described in claim 1, which is characterized in that compound concentration is the PCN solution conducts of 0.05 ~ 0.15 mg/ml
Fluorescence probe.
3. application as described in claim 1, which is characterized in that a concentration of 0.05 μM ~ 10 μM of micro uric acid.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115805095A (en) * | 2022-12-12 | 2023-03-17 | 东南大学 | High-specific-surface-area porous composite photocatalyst, preparation method, integrated treatment system and treatment method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103301867A (en) * | 2013-06-25 | 2013-09-18 | 重庆工商大学 | Inorganic ion doped carbon nitride photocatalyst and preparation method thereof |
| CN106006581A (en) * | 2016-05-20 | 2016-10-12 | 太原理工大学 | Method for solvothermal preparation of fluorescent carbon nitride quantum dots |
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- 2017-04-11 CN CN201710230495.0A patent/CN108693150A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103301867A (en) * | 2013-06-25 | 2013-09-18 | 重庆工商大学 | Inorganic ion doped carbon nitride photocatalyst and preparation method thereof |
| CN106006581A (en) * | 2016-05-20 | 2016-10-12 | 太原理工大学 | Method for solvothermal preparation of fluorescent carbon nitride quantum dots |
Non-Patent Citations (2)
| Title |
|---|
| QIUJUN LU，ET.AL.: ""One-step electrochemical synthesis of ultrathin graphitic carbon nitride nanosheets and their application to the detection of uric acid"", 《CHEMICAL COMMUNICATION》 * |
| 郭欣荣: ""钼、钨及石墨相碳化氮二维层状材料的制备以及在分析检测中的某些应用"", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115805095A (en) * | 2022-12-12 | 2023-03-17 | 东南大学 | High-specific-surface-area porous composite photocatalyst, preparation method, integrated treatment system and treatment method |
| CN115805095B (en) * | 2022-12-12 | 2024-02-06 | 东南大学 | High specific surface area porous composite photocatalyst, preparation method, integrated treatment system and treatment method |
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Application publication date: 20181023 |