CN108982481A - A kind of preparation method and application of the electrochemical luminescence sensor based on the titanium doped bromine oxygen bismuth microballoon of golden functionalization - Google Patents
A kind of preparation method and application of the electrochemical luminescence sensor based on the titanium doped bromine oxygen bismuth microballoon of golden functionalization Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method and applications of electrochemical luminescence sensor based on the titanium doped bromine oxygen bismuth microballoon of golden functionalization, belong to electrochemical analysis and field of biosensors.Titanium doped bromine oxygen bismuth microballoon prepared by the present invention has big specific surface area and stable electrochemical luminescence signals.After gold nanoparticle functionalization, electric conductivity is improved, and electrochemical luminescence signals further enhance.The present invention is prepared for a kind of unmarked type electrochemical luminescence sensor using the titanium doped bromine oxygen bismuth of golden functionalization as luminescent material and substrate, and for the Sensitive Detection of N- akrencephalon pro-BNP, the range of linearity is 1 pgmL‑1‑50 ng·mL‑1, detect and be limited to 0.33 pgmL‑1。
Description
Technical field
The present invention relates to a kind of preparation sides of electrochemical luminescence sensor based on the titanium doped bromine oxygen bismuth microballoon of golden functionalization
Method and application.A kind of detection is specifically prepared for as luminescent material and substrate using the golden titanium doped bromine oxygen bismuth microballoon of functionalization
The unmarked type electrochemical luminescence sensor of N- akrencephalon pro-BNP, belongs to electrochemical analysis and field of biosensors.
Background technique
Heart failure is most severe one of the health problem in the whole world, and the whole world has more than 2,300 ten thousand people with heart failure.The heart
The disease incidence to decline increases year by year, forces us that must pay attention to heart failure early stage correct diagnosing and treating, to extend the longevity of patient
It orders, improve its quality of life.The index most sensitive and special as cardiac disorder, N- akrencephalon pro-BNP is in heart failure
There is important value in screening, curative effect evaluation and Index for diagnosis.How to realize quasi- to the efficient and sensible of N- akrencephalon pro-BNP
Really detecting is current urgent problem to be solved.
The analysis method of detection N- akrencephalon pro-BNP mainly has radioimmunoassay method and enzyme-linked immunosorbent assay at present,
Although both methods has certain superiority, there is also apparent limitations, and wherein radioimmunoassay method exists and puts
The problems such as injectivity waste processing, the device is complicated, and the enzyme-linked immunosorbent assay measurement period is long, reproducibility is poor, sensitivity is lower.For
The drawbacks of overcoming the above traditional analysis, the present invention be prepared for it is a kind of it is easy to operate quickly, the electrochemistry of high sensitivity hair
Optical sensor is used for the detection of N- akrencephalon pro-BNP.
Electrochemical luminescence is the chemiluminescence phenomenon directly or indirectly caused by electrochemical reaction, as electrochemistry and chemistry
The product of the luminous infiltration that crosses one another, the hypersensitivity of the existing luminesceence analysis of this method, and it is controllable to combine electrochemical potentials
The advantages of, so causing the great attention of the numerous areas such as analytical chemistry and bioanalysis.Currently used for detecting N- akrencephalon sodium
The electrochemical luminescence sensor of peptide precursor is to be based on interlayer type immune sensing strategy mostly, sensing strategy markers step complexity,
The costly and time consuming length of experimental cost.Based on this, the present invention is prepared for a kind of electrochemistry of unmarked type detection N- akrencephalon pro-BNP
Luminescence sensor, the sensor have many advantages, such as that preparation is simple, response is rapid, cost is relatively low.
Conventional electrochemical luminescent material such as luminol, tris (bipyridine) ruthenium etc. has in fixed difficult, the luminous letter of electrode surface
The disadvantages of number unstable.Therefore, the present invention is prepared for a kind of titanium doped bromine oxygen bismuth microballoon of golden functionalization, and finds that the material can
It generates stable electrochemical luminescence signals and is easily fastened to electrode surface, application of the material in electrochemical luminescence sensor
It still belongs to the first time.Titanium doped bromine oxygen bismuth microballoon prepared by the present invention has big specific surface area and stable electrochemical luminescence signals.
With gold nanoparticle by after its functionalization, the electric conductivity of the golden titanium doped bromine oxygen bismuth microballoon of functionalization is improved, electrochemical luminescence signals
It further enhances, electrochemical luminescence signals are twice or more of titanium doped bromine oxygen bismuth microballoon.The present invention mixes golden functionalization titanium
Miscellaneous bromine oxygen bismuth microballoon is prepared for a kind of unmarked type electrochemical luminescence sensor as luminescent material and substrate, is used for N- akrencephalon
The Sensitive Detection of pro-BNP.Electrochemical luminescence sensor prepared by the present invention is 1 to the detection range of N- akrencephalon pro-BNP
pg·mL-1-50 ng·mL-1, detection, which limits, reaches 0.33 pgmL-1.The sensor can be effectively used for N- akrencephalon pro-BNP
Analysis detection, has many advantages, such as to prepare that simple and quick, analysis cost is low, high sensitivity.
Summary of the invention
An object of the present invention is to synthesize flower-shaped titanium doped bromine oxygen bismuth microballoon and as electrochemical luminescence material.Flower
Shape bromine oxygen bismuth microballoon has biggish specific surface area, and the doping of titanium increases its specific surface area, and forms hetero-junctions at interface.
The second object of the present invention is to gold nanoparticle by titanium doped bromine oxygen bismuth microballoon functionalization to improve its electric conductivity.
Gold nanoparticle improves the electric conductivity of titanium doped bromine oxygen bismuth microballoon, in addition, gold nanoparticle has good biocompatibility,
It can be connect by gold-ammonia key with antibody.
The third object of the present invention is to provide a kind of preparation method of simple and easy N- akrencephalon pro-BNP sensor.It will
The golden titanium doped bromine oxygen bismuth microballoon of functionalization does not need complicated cumbersome labelling technique, can be realized as luminescent material and substrate
Rapid sensitive detection to N- akrencephalon pro-BNP.
To achieve the goals above, The technical solution adopted by the invention is as follows:
1. a kind of preparation method and application of the electrochemical luminescence sensor based on the titanium doped bromine oxygen bismuth microballoon of golden functionalization,
It is characterized in that, comprising the following steps:
(1) by glass-carbon electrode alumina powder sanding and polishing that diameter is 4 mm to mirror surface, then it is clean with milli-Q water；
It (2) is 4~14 mgmL by 6 μ L, concentration-1The water-soluble drop-coated of the golden titanium doped bromine oxygen bismuth microballoon of functionalization is to electrode
Surface, room temperature preservation to drying；
(3) 6 μ L of drop coating, concentration are 2~14 μ gmL-1N- akrencephalon pro-BNP antibody-solutions in glassy carbon electrode surface,
It is saved at 4 DEG C to drying, ultrapure water cleaning；
(4) 3 μ L of drop coating, the bovine serum albumin(BSA) that mass fraction is 1%, close nonspecific activity site, save at 4 DEG C to
It is dry, ultrapure water cleaning；
It (5) is 0.001-50 ngmL by 6 μ L, concentration-1A series of various concentrations N- akrencephalon pro-BNP drop coating in electricity
Pole surface saves the electrochemical luminescence sensing that detection N- akrencephalon pro-BNP is obtained to drying, ultrapure water cleaning at 4 DEG C
Device.
2. a kind of electrochemical luminescence sensing based on the titanium doped bromine oxygen bismuth microballoon of golden functionalization as described in claim 1
The preparation method and application of device, the titanium doped bromine oxygen bismuth microballoon of the gold functionalization, which is characterized in that preparation step is as follows:
(1) preparation of titanium doped bromine oxygen bismuth microballoon
By 0.4~0.8 g Bi (NO3)3·5H2O is dissolved into 60 mL 2-methyl cellosolves, and it is molten that stirring forms it into clarification
Liquid is then slowly added into 1.2 g cetyl trimethylammonium bromides and 0.3 mL butyl titanate, will after 30 min of magnetic agitation
Above-mentioned solution is transferred in reaction kettle, 160 DEG C of 24 h of reaction.It after being cooled to room temperature, is centrifuged, washs, being dried to obtain titanium doped bromine
Oxygen bismuth microballoon；
(2) preparation of the titanium doped bromine oxygen bismuth microballoon of golden functionalization
The titanium doped bromine oxygen bismuth microballoon of the above-mentioned preparation of 0.3~0.5 g is distributed in 100 mL ultrapure waters, after 1 h of ultrasound, uses ammonia
Water adjusts pH value of solution to 11.By 5 mL, the HAuCl that mass fraction is 1%4It is added dropwise in above-mentioned solution, magnetic force at 50 DEG C
5 h are stirred, obtain the titanium doped bromine oxygen bismuth microballoon of golden functionalization after centrifugation, washing, drying.
3. electrochemical luminescence sensor as described in claim 1 is used for the detection of N- akrencephalon pro-BNP, feature exists
In steps are as follows:
(1) using Ag/AgCl electrode as reference electrode, platinum electrode as to electrode, obtained electrochemical luminescence sensor
It as working electrode, is connected in the magazine of chemiluminescence detector, electrochemical workstation is connected with chemiluminescence detector
Together；
(2) chemiluminescence detector parameter is set as, and the high pressure of photomultiplier tube is set as 750 V, and sweep speed is set as 0.1
V/s；
(3) electrochemical workstation parameter is set as, and cyclic voltammetry scan potential range is -1.8~0 V, and sweep speed is set as
0.1 V/s；
(4) using containing 100 mM KCl and 40~140 mM K2S2O8PBS buffer solution as test bottom liquid, pass through electrochemistry
Luminescence method detects the electrochemical luminescence signals intensity that the N- akrencephalon pro-BNP of various concentration generates；The PBS buffer solution,
PH=5.5~8.5, with 0.1 M Na2HPO4With 0.1 M KH2PO4It prepares；
(5) according to the linear relationship of resulting electrochemical luminescence intensity value and N- akrencephalon pro-BNP log concentration, work is drawn
Curve.
Beneficial achievement of the invention
(1) present invention makes the specific surface area of bromine oxygen bismuth microballoon by 11.55 m using the doping of titanium2/ g increases to 109.2 m2/ g,
Interface hetero-junctions is formd between titanium and bromine oxygen bismuth simultaneously, the band gap of bromine oxygen bismuth is reduced, so that the electrochemical luminescence of bromine oxygen bismuth
Enhanced strength, application of the titanium doped bromine oxygen bismuth microballoon in electrochemical luminescence sensor still belong to the first time；
(2) titanium doped bromine oxygen bismuth microballoon prepared by the present invention have big specific surface area, can with immobilized a large amount of gold nanoparticle,
To combine more antibody, while gold nanoparticle improves the electric conductivity of base material, further enhances electrochemistry hair
Optical signal, the electrochemical luminescence signals of the golden titanium doped bromine oxygen bismuth microballoon of functionalization are twice or more of titanium doped bromine oxygen bismuth microballoon；
(3) present invention is prepared for unmarked using the titanium doped bromine oxygen bismuth microballoon of golden functionalization as electrochemical luminescence material and substrate
Type electrochemical luminescence sensor is used for the detection of N- akrencephalon pro-BNP.The sensor operations are simple, are swift in response, and may be implemented
Highly selective and highly sensitive detection to N- akrencephalon pro-BNP.Sensor prepared by the present invention detects N- akrencephalon pro-BNP
The range of linearity be 1 pgmL-1-50 ng·mL-1, detect and be limited to 0.33 pgmL-1。
Specific embodiment
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 1
1. a kind of preparation method of the electrochemical luminescence sensor based on the titanium doped bromine oxygen bismuth microballoon of golden functionalization
(1) preparation of titanium doped bromine oxygen bismuth microballoon
By 0.4 g Bi (NO3)3·5H2O is dissolved into 60 mL 2-methyl cellosolves, and stirring forms it into clear solution, then
1.2 g cetyl trimethylammonium bromides and 0.3 mL butyl titanate are slowly added to, it will be above-mentioned molten after 30 min of magnetic agitation
Liquid is transferred in reaction kettle, 160 DEG C of 24 h of reaction.It after being cooled to room temperature, is centrifuged, washs, to be dried to obtain titanium doped bromine oxygen bismuth micro-
Ball.
(2) preparation of the titanium doped bromine oxygen bismuth microballoon of golden functionalization
The titanium doped bromine oxygen bismuth microballoon of the above-mentioned preparation of 0.3 g is distributed in 100 mL ultrapure waters, after 1 h of ultrasound, with ammonium hydroxide tune
PH value of solution is saved to 11.By 5 mL, the HAuCl that mass fraction is 1%4It is added dropwise in above-mentioned solution, magnetic agitation 5 at 50 DEG C
H obtains the titanium doped bromine oxygen bismuth microballoon of golden functionalization after centrifugation, washing, drying.
(3) preparation of electrochemical luminescence sensor
1) by glass-carbon electrode alumina powder sanding and polishing that diameter is 4 mm to mirror surface, then it is clean with milli-Q water；
It 2) is 4 mgmL by 6 μ L, concentration-1The water-soluble drop-coated of the golden titanium doped bromine oxygen bismuth microballoon of functionalization to electrode surface,
Room temperature preservation is to drying；
3) 6 μ L of drop coating, concentration are 6 μ gmL-1N- akrencephalon pro-BNP antibody-solutions in glassy carbon electrode surface, 4 DEG C
It is lower to save to drying, ultrapure water cleaning；
4) 3 μ L of drop coating, the bovine serum albumin(BSA) that mass fraction is 1% close nonspecific activity site, are saved at 4 DEG C to dry
It is dry, ultrapure water cleaning；
It 5) is 0.001-50 ngmL by 6 μ L, concentration-1A series of various concentrations N- akrencephalon pro-BNP drop coating in electricity
Pole surface saves at 4 DEG C to drying, ultrapure water cleaning.
2. the electrochemical luminescence sensor is applied to the detection to N- akrencephalon pro-BNP
(1) using Ag/AgCl electrode as reference electrode, platinum electrode as to electrode, obtained electrochemical luminescence sensor
It as working electrode, is connected in the magazine of chemiluminescence detector, electrochemical workstation is connected with chemiluminescence detector
Together；
(2) chemiluminescence detector parameter is set as, and the high pressure of photomultiplier tube is set as 750 V, and sweep speed is set as 0.1
V/s；
(3) electrochemical workstation parameter is set as, and cyclic voltammetry scan potential range is -1.8~0 V, and sweep speed is set as
0.1 V/s；
(4) using containing 100 mM KCl and 40~140 mM K2S2O8PBS buffer solution as test bottom liquid, pass through electrochemistry
Luminescence method detects the electrochemical luminescence signals intensity that the N- akrencephalon pro-BNP of various concentration generates；The PBS buffer solution,
PH=5.5~8.5, with 0.1 M Na2HPO4With 0.1 M KH2PO4It prepares；
(5) according to the linear relationship of resulting electrochemical luminescence intensity value and N- akrencephalon pro-BNP log concentration, work is drawn
Curve.
Embodiment 2
1. a kind of preparation method of the electrochemical luminescence sensor based on the titanium doped bromine oxygen bismuth microballoon of golden functionalization
(1) preparation of titanium doped bromine oxygen bismuth microballoon
By 0.5 g Bi (NO3)3·5H2O is dissolved into 60 mL 2-methyl cellosolves, and stirring forms it into clear solution, then
1.2 g cetyl trimethylammonium bromides and 0.3 mL butyl titanate are slowly added to, it will be above-mentioned molten after 30 min of magnetic agitation
Liquid is transferred in reaction kettle, 160 DEG C of 24 h of reaction.It after being cooled to room temperature, is centrifuged, washs, to be dried to obtain titanium doped bromine oxygen bismuth micro-
Ball.
(2) preparation of the titanium doped bromine oxygen bismuth microballoon of golden functionalization
The titanium doped bromine oxygen bismuth microballoon of the above-mentioned preparation of 0.5 g is distributed in 100 mL ultrapure waters, after 1 h of ultrasound, with ammonium hydroxide tune
PH value of solution is saved to 11.By 5 mL, the HAuCl that mass fraction is 1%4It is added dropwise in above-mentioned solution, magnetic agitation 5 at 50 DEG C
H obtains the titanium doped bromine oxygen bismuth microballoon of golden functionalization after centrifugation, washing, drying.
(3) preparation of electrochemical luminescence sensor
1) by glass-carbon electrode alumina powder sanding and polishing that diameter is 4 mm to mirror surface, then it is clean with milli-Q water；
It 2) is 10 mgmL by 6 μ L, concentration-1The water-soluble drop-coated of the golden titanium doped bromine oxygen bismuth microballoon of functionalization to electrode surface,
Room temperature preservation is to drying；
3) 6 μ L of drop coating, concentration are 6 μ gmL-1N- akrencephalon pro-BNP antibody-solutions in glassy carbon electrode surface, 4 DEG C
It is lower to save to drying, ultrapure water cleaning；
4) 3 μ L of drop coating, the bovine serum albumin(BSA) that mass fraction is 1% close nonspecific activity site, are saved at 4 DEG C to dry
It is dry, ultrapure water cleaning；
It 5) is 0.001-50 ngmL by 6 μ L, concentration-1A series of various concentrations N- akrencephalon pro-BNP drop coating in electricity
Pole surface saves at 4 DEG C to drying, ultrapure water cleaning.
2. the electrochemical luminescence sensor is applied to the detection to N- akrencephalon pro-BNP
(1) using Ag/AgCl electrode as reference electrode, platinum electrode as to electrode, obtained electrochemical luminescence sensor
It as working electrode, is connected in the magazine of chemiluminescence detector, electrochemical workstation is connected with chemiluminescence detector
Together；
(2) chemiluminescence detector parameter is set as, and the high pressure of photomultiplier tube is set as 750 V, and sweep speed is set as 0.1
V/s；
(3) electrochemical workstation parameter is set as, and cyclic voltammetry scan potential range is -1.8~0 V, and sweep speed is set as
0.1 V/s；
(4) using containing 100 mM KCl and 40~140 mM K2S2O8PBS buffer solution as test bottom liquid, pass through electrochemistry
Luminescence method detects the electrochemical luminescence signals intensity that the N- akrencephalon pro-BNP of various concentration generates；The PBS buffer solution,
PH=5.5~8.5, with 0.1 M Na2HPO4With 0.1 M KH2PO4It prepares；
(5) according to the linear relationship of resulting electrochemical luminescence intensity value and N- akrencephalon pro-BNP log concentration, work is drawn
Curve.
Embodiment 3
1. a kind of preparation method of the electrochemical luminescence sensor based on the titanium doped bromine oxygen bismuth microballoon of golden functionalization
(1) preparation of titanium doped bromine oxygen bismuth microballoon
By 0.8 g Bi (NO3)3·5H2O is dissolved into 60 mL 2-methyl cellosolves, and stirring forms it into clear solution, then
1.2 g cetyl trimethylammonium bromides and 0.3 mL butyl titanate are slowly added to, it will be above-mentioned molten after 30 min of magnetic agitation
Liquid is transferred in reaction kettle, 160 DEG C of 24 h of reaction.It after being cooled to room temperature, is centrifuged, washs, to be dried to obtain titanium doped bromine oxygen bismuth micro-
Ball.
(2) preparation of the titanium doped bromine oxygen bismuth microballoon of golden functionalization
The titanium doped bromine oxygen bismuth microballoon of the above-mentioned preparation of 0.4 g is distributed in 100 mL ultrapure waters, after 1 h of ultrasound, with ammonium hydroxide tune
PH value of solution is saved to 11.By 5 mL, the HAuCl that mass fraction is 1%4It is added dropwise in above-mentioned solution, magnetic agitation 5 at 50 DEG C
H obtains the titanium doped bromine oxygen bismuth microballoon of golden functionalization after centrifugation, washing, drying.
(3) preparation of electrochemical luminescence sensor
1) by glass-carbon electrode alumina powder sanding and polishing that diameter is 4 mm to mirror surface, then it is clean with milli-Q water；
It 2) is 12 mgmL by 6 μ L, concentration-1The water-soluble drop-coated of the golden titanium doped bromine oxygen bismuth microballoon of functionalization to electrode surface,
Room temperature preservation is to drying；
3) 6 μ L of drop coating, concentration are 6 μ gmL-1N- akrencephalon pro-BNP antibody-solutions in glassy carbon electrode surface, 4 DEG C
It is lower to save to drying, ultrapure water cleaning；
4) 3 μ L of drop coating, the bovine serum albumin(BSA) that mass fraction is 1% close nonspecific activity site, are saved at 4 DEG C to dry
It is dry, ultrapure water cleaning；
It 5) is 0.001-50 ngmL by 6 μ L, concentration-1A series of various concentrations N- akrencephalon pro-BNP drop coating in electricity
Pole surface saves at 4 DEG C to drying, ultrapure water cleaning.
2. the electrochemical luminescence sensor is applied to the detection to N- akrencephalon pro-BNP
(1) using Ag/AgCl electrode as reference electrode, platinum electrode as to electrode, obtained electrochemical luminescence sensor
It as working electrode, is connected in the magazine of chemiluminescence detector, electrochemical workstation is connected with chemiluminescence detector
Together；
(2) chemiluminescence detector parameter is set as, and the high pressure of photomultiplier tube is set as 750 V, and sweep speed is set as 0.1
V/s；
(3) electrochemical workstation parameter is set as, and cyclic voltammetry scan potential range is -1.8~0 V, and sweep speed is set as
0.1 V/s；
(4) using containing 100 mM KCl and 40~140 mM K2S2O8PBS buffer solution as test bottom liquid, pass through electrochemistry
Luminescence method detects the electrochemical luminescence signals intensity that the N- akrencephalon pro-BNP of various concentration generates；The PBS buffer solution,
PH=5.5~8.5, with 0.1 M Na2HPO4With 0.1 M KH2PO4It prepares；
(5) according to the linear relationship of resulting electrochemical luminescence intensity value and N- akrencephalon pro-BNP log concentration, work is drawn
Curve.
Claims (3)
1. a kind of preparation method and application of the electrochemical luminescence sensor based on the titanium doped bromine oxygen bismuth microballoon of golden functionalization, special
Sign is, comprising the following steps:
(1) by glass-carbon electrode alumina powder sanding and polishing that diameter is 4 mm to mirror surface, then it is clean with milli-Q water；
It (2) is 4~14 mgmL by 6 μ L, concentration-1The water-soluble drop-coated of the golden titanium doped bromine oxygen bismuth microballoon of functionalization is to electrode table
Face, room temperature preservation to drying；
(3) 6 μ L of drop coating, concentration are 2~14 μ gmL-1N- akrencephalon pro-BNP antibody-solutions in glassy carbon electrode surface, 4
It is saved at DEG C to drying, ultrapure water cleaning；
(4) 3 μ L of drop coating, the bovine serum albumin(BSA) that mass fraction is 1%, close nonspecific activity site, save at 4 DEG C to
It is dry, ultrapure water cleaning；
It (5) is 0.001-50 ngmL by 6 μ L, concentration-1A series of various concentrations N- akrencephalon pro-BNP drop coating in electricity
Pole surface saves the electrochemical luminescence sensing that detection N- akrencephalon pro-BNP is obtained to drying, ultrapure water cleaning at 4 DEG C
Device.
2. a kind of system of the electrochemical luminescence sensor based on the titanium doped bromine oxygen bismuth microballoon of golden functionalization as described in claim 1
Preparation Method and application, the titanium doped bromine oxygen bismuth microballoon of the gold functionalization, which is characterized in that preparation step is as follows:
(1) preparation of titanium doped bromine oxygen bismuth microballoon
By 0.4~0.8 g Bi (NO3)3·5H2O is dissolved into 60 mL 2-methyl cellosolves, and it is molten that stirring forms it into clarification
Liquid is then slowly added into 1.2 g cetyl trimethylammonium bromides and 0.3 mL butyl titanate, will after 30 min of magnetic agitation
Above-mentioned solution is transferred in reaction kettle, 160 DEG C of 24 h of reaction；It after being cooled to room temperature, is centrifuged, washs, being dried to obtain titanium doped bromine
Oxygen bismuth microballoon；
(2) preparation of the titanium doped bromine oxygen bismuth microballoon of golden functionalization
The titanium doped bromine oxygen bismuth microballoon of the above-mentioned preparation of 0.3~0.5 g is distributed in 100 mL ultrapure waters, after 1 h of ultrasound, uses ammonia
Water adjusts pH value of solution to 11；By 5 mL, the HAuCl that mass fraction is 1%4It is added dropwise in above-mentioned solution, magnetic force at 50 DEG C
5 h are stirred, obtain the titanium doped bromine oxygen bismuth microballoon of golden functionalization after centrifugation, washing, drying.
3. the detection that electrochemical luminescence sensor as described in claim 1 is used for N- akrencephalon pro-BNP, which is characterized in that step
It is rapid as follows:
(1) using Ag/AgCl electrode as reference electrode, platinum electrode as to electrode, obtained electrochemical luminescence sensor
It as working electrode, is connected in the magazine of chemiluminescence detector, electrochemical workstation is connected with chemiluminescence detector
Together；
(2) chemiluminescence detector parameter is set as, and the high pressure of photomultiplier tube is set as 750 V, and sweep speed is set as 0.1
V/s；
(3) electrochemical workstation parameter is set as, and cyclic voltammetry scan potential range is -1.8~0 V, and sweep speed is set as
0.1 V/s；
(4) using containing 100 mM KCl and 40~140 mM K2S2O8PBS buffer solution as test bottom liquid, pass through electrochemistry
Luminescence method detects the electrochemical luminescence signals intensity that the N- akrencephalon pro-BNP of various concentration generates；The PBS buffer solution,
PH=5.5~8.5, with 0.1 M Na2HPO4With 0.1 M KH2PO4It prepares；
(5) according to the linear relationship of resulting electrochemical luminescence intensity value and N- akrencephalon pro-BNP log concentration, work is drawn
Curve.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111830102A (en) * | 2020-07-06 | 2020-10-27 | 济南大学 | Preparation method of electrochemical luminescence immunosensor for detecting CYFRA21-1 by copper-doped Tb-based MOF |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103487573A (en) * | 2013-09-27 | 2014-01-01 | 安徽大学 | Electrogenerated chemiluminescence immunosensor for detecting human interleukin 6 as well as preparation method and detection method of immunosensor |
| CN103611554A (en) * | 2013-12-02 | 2014-03-05 | 镇江市高等专科学校 | Preparation method of photocatalytic material titanium (Ti)-doped bismuth oxychloride (BiOCl) microsphere |
| CN104880456A (en) * | 2015-05-22 | 2015-09-02 | 济南大学 | Preparation method and application of electrochemiluminescence immunosensor constructed on basis of GO/MWCNTs-COOH/Au @ CeO2 |
| CN106442671A (en) * | 2016-09-12 | 2017-02-22 | 济南大学 | Preparation method of no-mark insulin sensor based on BiOBr/Ag2S composite material |
| CN106645094A (en) * | 2017-01-08 | 2017-05-10 | 济南大学 | Electrochemiluminescence sensor for detecting concanavalin A by using Fe3O4-supported Ru(bpy)3<2+> |
| CN107389773A (en) * | 2017-06-21 | 2017-11-24 | 陕西科技大学 | Graphene composite hollow bismuth oxybromide electrochemica biological sensor and preparation method thereof |
| CN107543851A (en) * | 2017-08-25 | 2018-01-05 | 济南大学 | A kind of preparation method and application of the electrochemical luminescence sensor based on silver oxalate bridging tris (bipyridine) ruthenium nano-complex |
| US20180120250A1 (en) * | 2015-04-08 | 2018-05-03 | Board Of Regents, The University Of Texas System | Methods and systems for the detection of analytes |
-
2018
- 2018-07-31 CN CN201810855921.4A patent/CN108982481A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103487573A (en) * | 2013-09-27 | 2014-01-01 | 安徽大学 | Electrogenerated chemiluminescence immunosensor for detecting human interleukin 6 as well as preparation method and detection method of immunosensor |
| CN103611554A (en) * | 2013-12-02 | 2014-03-05 | 镇江市高等专科学校 | Preparation method of photocatalytic material titanium (Ti)-doped bismuth oxychloride (BiOCl) microsphere |
| US20180120250A1 (en) * | 2015-04-08 | 2018-05-03 | Board Of Regents, The University Of Texas System | Methods and systems for the detection of analytes |
| CN104880456A (en) * | 2015-05-22 | 2015-09-02 | 济南大学 | Preparation method and application of electrochemiluminescence immunosensor constructed on basis of GO/MWCNTs-COOH/Au @ CeO2 |
| CN106442671A (en) * | 2016-09-12 | 2017-02-22 | 济南大学 | Preparation method of no-mark insulin sensor based on BiOBr/Ag2S composite material |
| CN106645094A (en) * | 2017-01-08 | 2017-05-10 | 济南大学 | Electrochemiluminescence sensor for detecting concanavalin A by using Fe3O4-supported Ru(bpy)3<2+> |
| CN107389773A (en) * | 2017-06-21 | 2017-11-24 | 陕西科技大学 | Graphene composite hollow bismuth oxybromide electrochemica biological sensor and preparation method thereof |
| CN107543851A (en) * | 2017-08-25 | 2018-01-05 | 济南大学 | A kind of preparation method and application of the electrochemical luminescence sensor based on silver oxalate bridging tris (bipyridine) ruthenium nano-complex |
Non-Patent Citations (1)
| Title |
|---|
| 马博凯: "溶剂热法制备BiOBr/Graphene和BiOBr/TiO2及其光催化性能研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111830102A (en) * | 2020-07-06 | 2020-10-27 | 济南大学 | Preparation method of electrochemical luminescence immunosensor for detecting CYFRA21-1 by copper-doped Tb-based MOF |
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