CN106198501B - A kind of preparation method for the Electrochemiluminescsensor sensor detecting aflatoxin - Google Patents
A kind of preparation method for the Electrochemiluminescsensor sensor detecting aflatoxin Download PDFInfo
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- CN106198501B CN106198501B CN201610521138.5A CN201610521138A CN106198501B CN 106198501 B CN106198501 B CN 106198501B CN 201610521138 A CN201610521138 A CN 201610521138A CN 106198501 B CN106198501 B CN 106198501B
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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
- G01N21/76—Chemiluminescence; Bioluminescence
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N27/28—Electrolytic cell components
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- G01N27/305—Electrodes, e.g. test electrodes; Half-cells optically transparent or photoresponsive electrodes
Abstract
The invention discloses a kind of preparation methods of electrogenerated chemiluminescence aflatoxin sensor.Belong to Nano-function thin films and biosensor technology field.The method comprises the steps of firstly, preparing a kind of New Two Dimensional nanocomposites, i.e. the two-dimensional nano composite material Mn-TiO of additive Mn nano titania square In-situ reaction molybdenum disulfide2/MoS2, good biocompatibility and big specific surface area using the material, aflatoxin antibody in load, when being detected, since additive Mn titanium dioxide can be with catalyzing hydrogen peroxide in-situ preparation O2, and with the K in the liquid of bottom2S2O8It is electrochemically reacted, generate electrochemiluminescence signal, recycle antibody in conjunction with the specific quantification of antigen to the influence of electron transport ability, so that current strength reduces, to reduce luminous intensity, the building of the Electrochemiluminescsensor sensor using unmarked electrogenerated chemiluminescence method detection aflatoxin is finally realized.
Description
Technical field
The present invention relates to a kind of preparation methods of electrogenerated chemiluminescence aflatoxin sensor.Belong to novel nanometer functional
Material and biosensor technology field.
Background technique
Aflatoxin is the similar compound of a kind of chemical structure, is the derivative of dihydrofuran cumarin.Huang Qu
Mould toxin is present in soil, animals and plants, in various nuts, is especially easy the grains such as pollution peanut, corn, rice, soybean, wheat
Oil product is mycotoxicosis maximum, to human health risk a kind of mycotoxin extremely outstanding.Aflatoxin master
There are Aflatoxins M1, aflatoxin B1, aflatoxin B 2, aflatoxin G 1, aflatoxin G 2 etc. several.It is yellow
It is 1 class carcinogenic substance that aspertoxin delimited by the World Health Organization, and toxicity is 68 times bigger than arsenic, is only second to meat poisoning mycin, is current
Known mycetism is strongest.The harmfulness of aflatoxin is to be woven with destruction to people and animal's liver group, seriously
When can lead to that liver cancer is even dead, and Homemade fermented food can also detect aflatoxin, especially high temperature and humidity area
Grain and oil and product kind recall rate are higher.
Currently, the method for detection aflatoxin mainly has chromatography, mass spectrography etc..Such method instrument is valuable, operates
Complexity, laboratory personnel just can be carried out detection after needing professional training.Therefore, research and development are at low cost, detect fast, high sensitivity, is special
The strong aflatoxin sensor of property is of great significance.
Electrochemiluminescsensor sensor due to its high sensitivity, specificity it is good, easy to operate the advantages that be widely used in
The fields such as clinical diagnosis, Pharmaceutical Analysis, environmental monitoring.The superior Electrochemiluminescsensor sensor of processability, most critical skill
Art is exactly the raising of the performances such as effective fixation and the reproducibility of luminous intensity and stability and immune molecule.Titanium dioxide is application
A kind of most commonly used photocatalyst material, since sheet-like titanium dioxide nanomaterial can expose more high miller index surfaces,
With higher photocatalytic activity, titanium dioxide nanoplate has application prospect preferably than nanoparticle, for titanium dioxide
The research of nanometer sheet is also concerned.Meanwhile titanium dioxide poorly conductive is also limited by single titanium dioxide nano material structure
The sensitivity for the Electrochemiluminescsensor sensor built is not generally high, is unfavorable for practical application.But on semiconductor nano material
Modification or compound special nano material can effectively improve the Resonance energy transfer of semiconductor surface, generate stronger shine
Intensity, and greatly improve detection sensitivity.Therefore, designing, preparing efficient, stable titanium dioxide nanoplate and its modifier is
Prepare the key technology of Electrochemiluminescsensor sensor.
Molybdenum disulfide (chemical formula MoS2) nano material, there is two-dimensional layered structure, be most widely used solid profit
One of lubrication prescription.Its sheet two-dimension nano materials after removing, is the semiconductor nano material haveing excellent performance, in addition to big ratio
Surface area, can be used as the carrier of catalyst and biological antibody, improve load capacity, while also have as co-catalyst excellent
Electron transmission performance.
Currently, most of synthesizing mean is all after being separately synthesized, then catalyst and carrier progress is compound, process is numerous
Trivial, yield is not high.Therefore, there is the two-dimensional nano composite material of excellent electrogenerated chemiluminescence performance to have In-situ reaction preparation
Have wide practical use and important scientific meaning.
Summary of the invention
The purpose of the present invention is to provide it is a kind of prepare simple, high sensitivity, detection quickly, the electroluminescent chemistry of high specificity
The preparation method of luminescence sensor, prepared sensor can be used for quick, the Sensitive Detection of aflatoxin.Based on this mesh
, the method comprises the steps of firstly, preparing a kind of New Two Dimensional nanocomposites, i.e. additive Mn nano titania square In-situ reaction
The two-dimensional nano composite material Mn-TiO of molybdenum disulfide2/MoS2, utilize the good biocompatibility and big ratio table of the material
Area, aflatoxin antibody in load, when being detected, since additive Mn titanium dioxide can be with catalyzing hydrogen peroxide original position
Generate O2, and with the K in the liquid of bottom2S2O8It is electrochemically reacted, generates electrochemiluminescence signal, recycle antibody and antigen
Specific quantification combine influence to electron transport ability it is final real to reduce luminous intensity so that current strength reduces
The building of the Electrochemiluminescsensor sensor using unmarked electrogenerated chemiluminescence method detection aflatoxin is showed.
The technical solution adopted by the invention is as follows:
1. a kind of preparation method for the Electrochemiluminescsensor sensor for detecting aflatoxin, it is characterised in that described
Electrochemiluminescsensor sensor is by working electrode, Mn-TiO2/MoS2, aflatoxin antibody, bovine serum albumin(BSA) composition；It is described
Mn-TiO2/MoS2For the two-dimensional nano composite material of additive Mn nano titania square In-situ reaction molybdenum disulfide；
It is characterized in that, the preparation method includes following preparation step:
A. Mn-TiO is prepared2/MoS2；
B. Electrochemiluminescsensor sensor is prepared；
Wherein, step a prepares Mn-TiO2/MoS2Specific steps are as follows:
(1) 0.6 g molybdenum disulfide powder and 0.2 ~ 2.0 mmol manganese salt is taken to be added to 3 ~ 10 mL n-BuLis jointly molten
In liquid, at nitrogen protection and 30 ~ 60 DEG C, stir 12 ~ 48 hours, the solution after being reacted；
(2) using the solution after reaction in nonpolar solvent washing step (1), water-bath is then carried out at 30 ~ 60 DEG C
Ultrasonic treatment, after handle, recycle nonpolar solvent carrying out washing treatment after solution, be dried in vacuo, obtain two sulphur of manganese intercalation
Change molybdenum nano material；
(3) the molybdenum disulfide nano material of manganese intercalation made from 10 ~ 500 mg steps (2) is taken to be added to 5 mL metatitanic acids four
In butyl ester, after stirring 1 hour, it is slowly added to 0.5 ~ 0.8 mL hydrofluoric acid while stirring, is then reacting at 160 ~ 180 DEG C
It is reacted 18 ~ 20 hours in kettle；
(4) by step (3) resulting reaction product, with ultrapure water and dehydrated alcohol centrifuge washing three times after, it is true at 50 DEG C
Sky is dry, obtains Mn-TiO2/MoS2；
The n-butyllithium solution is the hexane solution of n-BuLi, and concentration is 1.6 mol/L；
The manganese salt is selected from one of following: manganese sulfate, manganese chloride, manganese nitrate, organo-manganese compound；
The nonpolar solvent is selected from one of following: hexane, hexamethylene, carbon tetrachloride, benzene, toluene；
The water bath sonicator processing, processing time are 1 hour；
Step b prepares the specific steps of Electrochemiluminescsensor sensor are as follows:
(1) using ITO electro-conductive glass as working electrode, in the Mn-TiO of 8 ~ 12 μ L of electrode surface drop coating2/MoS2Colloidal sol, room
It is dried under temperature；
(2) electrode obtained in step (1) is cleaned with buffer solution PBS, is continued in 8 ~ 12 μ L of electrode surface drop coating
The aflatoxin antibody-solutions of 10 μ g/mL are saved in 4 DEG C of refrigerators and are dried；
(3) electrode obtained in step (2) is cleaned with PBS, continues in 8 ~ 12 μ L concentration of electrode surface drop coating to be 100
The bovine serum albumin solution of μ g/mL is saved in 4 DEG C of refrigerators and is dried；
(4) electrode obtained in step (3) is cleaned with PBS, saves after drying, obtains electroluminescent in 4 DEG C of refrigerators
Chemiluminescence sensor；
The Mn-TiO2/MoS2Colloidal sol is by the Mn-TiO of 50 mg2/MoS2Powder is dissolved in 10 mL ultrapure waters, and
The hydrosol obtained after 30 min of ultrasound；
The PBS is the phosphate buffer solution of 10 mmol/L, and the pH value of the phosphate buffer solution is 7.4.
2. the application of Electrochemiluminescsensor sensor prepared by preparation method of the present invention, which is characterized in that packet
Include following applying step:
A. standard solution is prepared: the aflatoxin standard for preparing one group of various concentration including blank standard specimen is molten
Liquid；
B. working electrode is modified: by Electrochemiluminescsensor sensor prepared by preparation method as described in claim 1
For working electrode, the aflatoxin standard solution for the various concentration prepared in step a is distinguished into drop coating to working electrode surface,
It is saved in 4 DEG C of refrigerators；
C. working curve is drawn: using Ag/AgCl electrode as reference electrode, platinum electrode is used as to electrode, with step b
The working electrode composition three-electrode system modified, is connected in electrochemiluminescdetection detection equipment；In a cell successively
The K of 15 mL is added2S2O8The H of solution and 100 μ L2O2Solution；Apply circulation electricity with working electrode of the cyclic voltammetry to assembling
Pressure；According to the relationship between the light signal strength of resulting electrogenerated chemiluminescence and aflatoxin antigen concentration of standard solution,
Draw working curve；The light signal strength of blank standard specimen is denoted asD 0, the light of the aflatoxin standard solution containing various concentration
Signal strength is denoted asD i, the difference that response light signal strength reduces is ΔD = D 0-D i, ΔDWith aflatoxin standard solution
Mass concentrationCBetween it is linear, draw ΔD?CWorking curve；
D. the detection of aflatoxin: the aflatoxin standard solution in step a is replaced with sample to be tested, according to step
Method in rapid b and c is detected, the difference DELTA that light signal strength reduces according to responseDAnd working curve, obtain sample to be tested
The content of middle aflatoxin；
The K2S2O8Solution is by 1 mol K2S2O8It is dissolved in the buffer solution of pH=6.5 of 10 L and making with 1 mol KCl
Standby to obtain, the buffer solution of the pH=6.5 is the phosphate buffer solution that pH value is 6.5；
The H2O2Solution is aqueous hydrogen peroxide solution, and the concentration of the aqueous hydrogen peroxide solution is 10%.
3. the preparation method and application of the Electrochemiluminescsensor sensor of detection aflatoxin of the present invention,
It is characterized in that the aflatoxin is selected from one of following: Aflatoxins M1, aflatoxin B1, aflatoxin
B2, aflatoxin G 1, aflatoxin G 2.
Beneficial achievement of the invention
(1) Electrochemiluminescsensor sensor preparation of the present invention is simple, easy to operate, realizes to aflatoxin
Quick, sensitive, highly selective detection, and it is at low cost, can be applied to portable inspectiont, there is market development prospect；
(2) present invention is prepared for New Two Dimensional nano material Mn-TiO using the method for In-situ reaction for the first time2/MoS2, the party
Method is mainly there are three advantage: first is that, it is sufficiently received with titanium dioxide due to growth in situ of the manganese on nano titania square
Rice square contact, is acted on using the metal surface plasma body of manganese, effectively increases semiconductor substrate Resonance energy transfer ability,
Although solving, titanium dioxide nanoplate specific surface area is bigger and mesoporous characteristic is suitable for electrogenerated chemiluminescence host material,
It is the unstable technical problem of electrochemiluminescence signal；Second is that the load due to molybdenum disulfide sheet two-dimension nano materials is special
Property and nano titania square on it fully dispersed, greatly increase electrogenerated chemiluminescence intensity, solve dioxy
Change titanium nanoplate difference and electrogenerated chemiluminescence intensity is weak and be unfavorable for preparing the technology of Electrochemiluminescsensor sensor and ask
Topic；Third is that finally using In-situ reaction since manganese ion is in this process not only as intercalation material but also as reaction dopant material
Method realize one pot of composite material preparation, not only save time, material loss, and make the additive Mn of preparation
Nano titania square can preferably evenly spread to above molybdenum disulfide sheet two-dimension nano materials.Therefore, the material
Effective preparation of material has important scientific meaning and application value；
(3) present invention is for the first time by Mn-TiO2/MoS2Applied in the preparation of electroluminescent chemiluminescence biosensor, significantly mention
The high strength and stability of electrogenerated chemiluminescence, substantially increases the detection sensitivity of Electrochemiluminescsensor sensor, so that
Electroluminescent chemiluminescence biosensor realizes application in actual operation；The application of the material is also associated biomolecule sensing
Device, such as optical electro-chemistry sensor, electrochemical sensor provide Technical Reference, have extensive potential use value.
Specific embodiment
1 Mn-TiO of embodiment2/MoS2Preparation
(1) 0.6 g molybdenum disulfide powder and 0.2 mmol manganese salt is taken to be added in 3mL n-butyllithium solution jointly, in nitrogen
At gas shielded and 60 DEG C, stir 12 hours, the solution after being reacted；
(2) using the solution after reaction in nonpolar solvent washing step (1), water bath sonicator is then carried out at 60 DEG C
Processing, after handle, recycle nonpolar solvent carrying out washing treatment after solution, be dried in vacuo, obtain the molybdenum disulfide of manganese intercalation
Nano material；
(3) the molybdenum disulfide nano material of manganese intercalation made from 500 mg steps (2) is taken to be added to 5 mL butyl titanates
In, after stirring 1 hour, it is slowly added to 0.5 mL hydrofluoric acid while stirring, then reacts in a kettle 18 hours at 160 DEG C；
(4) by step (3) resulting reaction product, with ultrapure water and dehydrated alcohol centrifuge washing three times after, it is true at 50 DEG C
Sky is dry, obtains Mn-TiO2/MoS2；
The n-butyllithium solution is the hexane solution of n-BuLi, and concentration is 1.6 mol/L；
The manganese salt is manganese sulfate；
The nonpolar solvent is hexane；
The water bath sonicator processing, processing time are 1 hour.
2 Mn-TiO of embodiment2/MoS2Preparation
(1) 0.6 g molybdenum disulfide powder and 1.0 mmol manganese salts is taken to be added in 5 mL n-butyllithium solutions jointly, in nitrogen
At gas shielded and 30 DEG C, stir 24 hours, the solution after being reacted；
(2) using the solution after reaction in nonpolar solvent washing step (1), water bath sonicator is then carried out at 30 DEG C
Processing, after handle, recycle nonpolar solvent carrying out washing treatment after solution, be dried in vacuo, obtain the molybdenum disulfide of manganese intercalation
Nano material；
(3) the molybdenum disulfide nano material of manganese intercalation made from 200 mg steps (2) is taken to be added to 5 mL butyl titanates
In, after stirring 1 hour, it is slowly added to 0.6 mL hydrofluoric acid while stirring, then reacts in a kettle 20 hours at 180 DEG C；
(4) by step (3) resulting reaction product, with ultrapure water and dehydrated alcohol centrifuge washing three times after, it is true at 50 DEG C
Sky is dry, obtains Mn-TiO2/MoS2；
The n-butyllithium solution is the hexane solution of n-BuLi, and concentration is 1.6 mol/L；
The manganese salt is manganese chloride；
The nonpolar solvent is carbon tetrachloride；
The water bath sonicator processing, processing time are 1 hour.
The preparation method of 3 Electrochemiluminescsensor sensor of embodiment
(1) using the ITO electro-conductive glass that width is 1 cm, a length of 4 cm as working electrode, 8 μ L's of electrode surface drop coating
Mn-TiO2/MoS2Colloidal sol dries at room temperature；
(2) electrode obtained in step (1) is cleaned with buffer solution PBS, is continued in 8 μ L of electrode surface drop coating, 10 μ
The aflatoxin antibody-solutions of g/mL are saved in 4 DEG C of refrigerators and are dried；
(3) electrode obtained in step (2) is cleaned with PBS, continues in 8 μ L concentration of electrode surface drop coating to be 100 μ
The bovine serum albumin solution of g/mL is saved in 4 DEG C of refrigerators and is dried；
(4) electrode obtained in step (3) is cleaned with PBS, is saved in 4 DEG C of refrigerators after drying, obtains electroluminescentization
Learn luminescence sensor；
The Mn-TiO2/MoS2Colloidal sol is by the Mn-TiO of 50 mg2/MoS2Powder is dissolved in 10 mL ultrapure waters, and
The hydrosol obtained after 30 min of ultrasound；
The PBS is the phosphate buffer solution of 10mmol/L, and the pH value of the phosphate buffer solution is 7.4,
The aflatoxin is aflatoxin B1.
The preparation method of 4 Electrochemiluminescsensor sensor of embodiment
(1) using the ITO electro-conductive glass that width is 1 cm, a length of 4 cm as working electrode, 10 μ L's of electrode surface drop coating
Mn-TiO2/MoS2Colloidal sol dries at room temperature；
(2) electrode obtained in step (1) is cleaned with buffer solution PBS, is continued in 10 μ L 10 of electrode surface drop coating
The aflatoxin antibody-solutions of μ g/mL are saved in 4 DEG C of refrigerators and are dried；
(3) electrode obtained in step (2) is cleaned with PBS, continues in 10 μ L concentration of electrode surface drop coating to be 100 μ
The bovine serum albumin solution of g/mL is saved in 4 DEG C of refrigerators and is dried；
(4) electrode obtained in step (3) is cleaned with PBS, saves after drying, obtains electroluminescent in 4 DEG C of refrigerators
Chemiluminescence sensor；
The Mn-TiO2/MoS2Colloidal sol is by the Mn-TiO of 50 mg2/MoS2Powder is dissolved in 10 mL ultrapure waters, and
The hydrosol obtained after 30 min of ultrasound；
The PBS is the phosphate buffer solution of 10 mmol/L, and the pH value of the phosphate buffer solution is 7.4,
The aflatoxin is Aflatoxins M1.
The preparation method of 5 Electrochemiluminescsensor sensor of embodiment
(1) using the ITO electro-conductive glass that width is 1 cm, a length of 4 cm as working electrode, 12 μ L's of electrode surface drop coating
Mn-TiO2/MoS2Colloidal sol dries at room temperature；
(2) electrode obtained in step (1) is cleaned with buffer solution PBS, is continued in 12 μ L 10 of electrode surface drop coating
The aflatoxin antibody-solutions of μ g/mL are saved in 4 DEG C of refrigerators and are dried；
(3) electrode obtained in step (2) is cleaned with PBS, continues in 12 μ L concentration of electrode surface drop coating to be 100 μ
The bovine serum albumin solution of g/mL is saved in 4 DEG C of refrigerators and is dried；
(4) electrode obtained in step (3) is cleaned with PBS, saves after drying, obtains electroluminescent in 4 DEG C of refrigerators
Chemiluminescence sensor；
The Mn-TiO2/MoS2Colloidal sol is by the Mn-TiO of 50 mg2/MoS2Powder is dissolved in 10 mL ultrapure waters, and
The hydrosol obtained after 30 min of ultrasound；
The PBS is the phosphate buffer solution of 10 mmol/L, and the pH value of the phosphate buffer solution is 7.4,
The aflatoxin is aflatoxin G 1.
The Electrochemiluminescsensor sensor of 6 embodiment 1 ~ 5 of embodiment preparation, applied to the detection of aflatoxin, step
It is rapid as follows:
(1) standard solution is prepared: the aflatoxin standard for preparing one group of various concentration including blank standard specimen is molten
Liquid；
(2) working electrode is modified: by Electrochemiluminescsensor sensor prepared by preparation method as described in claim 1
For working electrode, the aflatoxin standard solution for the various concentration prepared in step (1) is distinguished into drop coating to working electrode table
Face saves in 4 DEG C of refrigerators；
(3) working curve is drawn: using saturated calomel electrode as reference electrode, platinum electrode is as auxiliary electrode, with step
Suddenly the working electrode that (2) have been modified forms three-electrode system, is connected in electrochemiluminescdetection detection equipment；In a cell
The K of 15 mL is successively added2S2O8The H of solution and 100 μ L2O2Solution；It is followed with working electrode application of the cyclic voltammetry to assembling
Loop voltag；According to the pass between the light signal strength of resulting electrogenerated chemiluminescence and aflatoxin antigen concentration of standard solution
Working curve is drawn by system；The light signal strength of blank standard specimen is denoted asD 0, the aflatoxin standard solution containing various concentration
Light signal strength is denoted asD i, the difference that response light signal strength reduces is ΔD = D 0-D i, ΔDWith aflatoxin standard solution
Mass concentrationCBetween it is linear, draw ΔD?CWorking curve；The linear detection range of aflatoxin are as follows: 0.003
~ 100 ng/mL, detection limit are as follows: 1.1 pg/mL；
(4) detection of aflatoxin: the aflatoxin standard solution in step a is replaced with sample to be tested, according to step
Method in rapid b and c is detected, the difference DELTA that light signal strength reduces according to responseDAnd working curve, obtain sample to be tested
The content of middle aflatoxin；
The K2S2O8Solution is by 1 mol K2S2O8It is dissolved in the buffer solution of pH=6.5 of 10 L and making with 1 mol KCl
Standby to obtain, the buffer solution of the pH=6.5 is the phosphate buffer solution that pH value is 6.5；
The H2O2Solution is aqueous hydrogen peroxide solution, and the concentration of the aqueous hydrogen peroxide solution is 10%.
Claims (1)
1. a kind of preparation method for the Electrochemiluminescsensor sensor for detecting aflatoxin, it is characterised in that electroluminescentization
Luminescence sensor is learned by working electrode, Mn-TiO2/MoS2, aflatoxin antibody, bovine serum albumin(BSA) composition；The Mn-
TiO2/MoS2For the two-dimensional nano composite material of additive Mn nano titania square In-situ reaction molybdenum disulfide；
The Mn-TiO2/MoS2Specific preparation step are as follows: take 0.6 g molybdenum disulfide powder and 0.2 ~ 2.0 mmol manganese salt
It is added in 3 ~ 10 mL n-butyllithium solutions jointly, at nitrogen protection and 30 ~ 60 DEG C, stirs 12 ~ 48 hours, obtain
Solution after reaction；Water bath sonicator processing is carried out at 30 ~ 60 DEG C, after having handled, recycles nonpolar solvent carrying out washing treatment
Solution afterwards, vacuum drying, obtains the molybdenum disulfide nano material of manganese intercalation；Take two of manganese intercalation made from 10 ~ 500 mg
Molybdenum sulfide nano material is added in 5 mL butyl titanates, after stirring 1 hour, is slowly added to 0.5 ~ 0.8 mL while stirring
Then hydrofluoric acid reacts 18 ~ 20 hours at 160 ~ 180 DEG C in a kettle；Resulting reaction product, with ultrapure water and nothing
Water-ethanol centrifuge washing three times after, be dried in vacuo at 50 DEG C, obtain Mn-TiO2/MoS2；
The n-butyllithium solution is the hexane solution of n-BuLi, and concentration is 1.6 mol/L；
The manganese salt is selected from one of following: manganese sulfate, manganese chloride, manganese nitrate, organo-manganese compound；
The nonpolar solvent is selected from one of following: hexane, hexamethylene, carbon tetrachloride, benzene, toluene；
The water bath sonicator processing, processing time are 1 hour；
The specific preparation step of the Electrochemiluminescsensor sensor are as follows:
(1) using ITO electro-conductive glass as working electrode, in the Mn-TiO of 8 ~ 12 μ L of electrode surface drop coating2/MoS2Colloidal sol, at room temperature
It dries；
(2) electrode obtained in step (1) is cleaned with buffer solution PBS, is continued in 8 ~ 12 μ L of electrode surface drop coating, 10 μ
The aflatoxin antibody-solutions of g/mL are saved in 4 DEG C of refrigerators and are dried；
(3) electrode obtained in step (2) is cleaned with PBS, continues in 8 ~ 12 μ L concentration of electrode surface drop coating to be 100 μ g/
The bovine serum albumin solution of mL is saved in 4 DEG C of refrigerators and is dried；
(4) electrode obtained in step (3) is cleaned with PBS, is saved in 4 DEG C of refrigerators after drying, obtains electroluminescent chemistry
Luminescence sensor；
The Mn-TiO2/MoS2Colloidal sol is by the Mn-TiO of 50 mg2/MoS2Powder is dissolved in 10 mL ultrapure waters, and ultrasound
The hydrosol obtained after 30 min；
The PBS is the phosphate buffer solution of 10 mmol/L, and the pH value of the phosphate buffer solution is 7.4；
The aflatoxin is selected from one of following: Aflatoxins M1, aflatoxin B1, aflatoxin B 2, Huang Qu
Mould toxin G1, aflatoxin G 2.
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| CN107478698B (en) * | 2017-08-03 | 2019-08-20 | 山东理工大学 | A kind of preparation method and application of in-situ preparation silver sulfide competitive type aflatoxin optical electro-chemistry sensor |
| CN108845015B (en) * | 2018-06-28 | 2020-09-01 | 济南大学 | Preparation method and application of photoelectrochemical aflatoxin B1 sensor based on tungsten trioxide composite material |
| CN110530853B (en) * | 2019-09-16 | 2021-09-21 | 南京工业大学 | Method for detecting aflatoxin B1 based on visual BPE-ECL technology |
| CN112782155B (en) * | 2020-12-04 | 2022-06-28 | 北京交通大学 | Preparation method and application of electrochemiluminescence aflatoxin biosensor |
| CN112924662A (en) * | 2021-01-27 | 2021-06-08 | 齐鲁工业大学 | Preparation method of electrochemiluminescence immunosensor and application of electrochemiluminescence immunosensor in detection of aflatoxin B1 |
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