CN106198657A - A kind of preparation method of the parathion sensor built based on two-dimension nano materials - Google Patents
A kind of preparation method of the parathion sensor built based on two-dimension nano materials Download PDFInfo
- Publication number
- CN106198657A CN106198657A CN201610521134.7A CN201610521134A CN106198657A CN 106198657 A CN106198657 A CN 106198657A CN 201610521134 A CN201610521134 A CN 201610521134A CN 106198657 A CN106198657 A CN 106198657A
- Authority
- CN
- China
- Prior art keywords
- parathion
- solution
- preparation
- mos
- tio
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention discloses the preparation method of a kind of electrogenerated chemiluminescence parathion sensor.Belong to Nano-function thin films and biosensor technology field.The method comprises the steps of firstly, preparing the two-dimensional nano composite Co TiO of a kind of New Two Dimensional nano composite material titanium dioxide/molybdenum bisuphide composite, i.e. cobalt doped nano titania square In-situ reaction molybdenum bisuphide2/MoS2, utilizing the good biocompatibility of this material and big specific surface area, parathion antibody in load, when detecting, owing to cobalt doped titanium dioxide can be with catalyzing hydrogen peroxide in-situ preparation O2, and with the K in end liquid2S2O8It is electrochemically reacted, produce electrochemiluminescence signal, recycling antibody is combined the impact on electron transport ability with the specific quantification of antigen, current intensity is reduced, thus reduce luminous intensity, finally achieve the structure of the Electrochemiluminescsensor sensor using unmarked electrogenerated chemiluminescence method detection parathion.
Description
Technical field
The present invention relates to the preparation method of a kind of electrogenerated chemiluminescence parathion sensor.Belong to Nano-function thin films
With biosensor technology field.
Background technology
Parathion is a kind of broad spectrum activity height poison insecticide, have tag, stomach toxicity, fumigation action, and can penetrate into plant
In.Parathion to insecticide effect quickly, can be used for preventing and treating fruit tree pest insect and the wheat red mites etc. such as Cotton Gossypii, Fructus Mali pumilae, mandarin orange, pears, Fructus Persicae.
In soil, parathion slightly can be migrated to deep subsoil by the eluviation of water.Parathion in soil can be by planting
Thing root absorption and enter in plant.People eat by mistake this kind of plant or containing its residue plant after, parathion can pass through
Digestive tract, respiratory tract and complete skin and mucosa enter human body, it may appear that Nausea and vomiting, have a headache, have loose bowels, whole body weakness nothing
The preliminary symptom of poisoning such as power, is eaten for a long time or excess eats and can cause canceration.
At present, the method for detection parathion mainly has chromatography, mass spectrography etc..This type of method instrument is valuable, operation complexity,
Laboratory personnel just can detect after needing professional training.Therefore, R&D costs are low, it is fast, highly sensitive, high specificity to detect
Parathion sensor is significant.
Electrochemiluminescsensor sensor is widely used in due to advantages such as it are highly sensitive, specificity is good, easy and simple to handle
The fields such as clinical diagnosis, pharmaceutical analysis, environmental monitoring.The Electrochemiluminescsensor sensor that processability is superior, its most critical skill
Art is exactly the raising of the performances such as the most fixing and repeatability of luminous intensity and stability and immune molecule.Titanium dioxide is application
Most commonly used a kind of photocatalyst material, owing to sheet-like titanium dioxide nanomaterial can expose more high miller index surface,
Having higher photocatalytic activity, titanium dioxide nanoplate has ratio nanoparticle preferably application prospect, for titanium dioxide
The research of nanometer sheet also receives much concern.Meanwhile, titanium dioxide poorly conductive also limit by single titanium dioxide nano material structure
The sensitivity of the Electrochemiluminescsensor sensor built is the highest, is unfavorable for actual application.But, on semiconductor nano material
Modify or compound special nano material, the Resonance energy transfer of semiconductor surface can be effectively improved, produce higher luminescence
Intensity, and it is greatly improved detection sensitivity.Therefore, design, prepare efficient, stable titanium dioxide nanoplate and trim is
Prepare the key technology of Electrochemiluminescsensor sensor.
(chemical formula is MoS to molybdenum bisuphide2) nano material, there is two-dimensional layered structure, be most widely used solid profit
One of lubrication prescription.Lamellar two-dimension nano materials after its stripping, is the semiconductor nano material of excellent performance, except having big ratio
Surface area, can improve load capacity as catalyst and the carrier of biological antibody, also has simultaneously as promoter excellent
Electron transmission performance.
At present, most synthesizing mean be all be separately synthesized after, then catalyst is combined with carrier, process is numerous
Trivial, productivity is the highest.Therefore, In-situ reaction preparation is had to the two-dimensional nano composite tool of excellent electrogenerated chemiluminescence performance
Have wide practical use and important scientific meaning.
Summary of the invention
It is an object of the invention to provide a kind of prepare simple, highly sensitive, 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 parathion.Based on this purpose, this
First invention is prepared for a kind of New Two Dimensional nano composite material titanium dioxide/molybdenum bisuphide composite, i.e. cobalt doped
The two-dimensional nano composite Co-TiO of nano titania square In-situ reaction molybdenum bisuphide2/MoS2, utilize the good of this material
Good biocompatibility and big specific surface area, parathion antibody in load, when detecting, due to cobalt doped titanium dioxide
Can be with catalyzing hydrogen peroxide in-situ preparation O2, and with the K in end liquid2S2O8It is electrochemically reacted, produces electrogenerated chemiluminescence letter
Number, recycling antibody is combined the impact on electron transport ability with the specific quantification of antigen so that current intensity reduces, thus
Reduce luminous intensity, finally achieve and use the electrogenerated chemiluminescence of unmarked electrogenerated chemiluminescence method detection parathion to pass
The structure of sensor.
The technical solution used in the present invention is as follows:
1. the preparation method of parathion sensor built based on two-dimension nano materials, it is characterised in that described to sulfur
Phosphorus sensor is made up of working electrode, two-dimension nano materials, parathion antibody, bovine serum albumin;Described two-dimensional nano material
Material is the two-dimensional nano composite Co-TiO of cobalt doped nano titania square In-situ reaction molybdenum bisuphide2/MoS2;
It is characterized in that, described preparation method includes following preparation process:
A. Co-TiO is prepared2/MoS2;
B. parathion sensor is prepared;
Wherein, step a prepares Co-TiO2/MoS2Concretely comprise the following steps:
(1) take 0.6 g molybdenum disulfide powder and 0.2 ~ 2.0 mmol cobalt salt joins 3 ~ 10 mL n-butyllithium solutions jointly
In, at nitrogen protection and 30 ~ 60 DEG C, stir 12 ~ 48 hours, obtain reacted solution;
(2) utilize reacted solution in non-polar solven washing step (1), at 30 ~ 60 DEG C, then carry out water bath sonicator
Process, after having processed, the solution after recycling non-polar solven carrying out washing treatment, vacuum drying, obtain the molybdenum bisuphide of cobalt intercalation
Nano material;
(3) the molybdenum disulfide nano material taking the cobalt intercalation that 10 ~ 500 mg steps (2) prepare joins 5 mL butyl titanates
In, after stirring 1 hour, it is slowly added to 0.5 ~ 0.8 mL Fluohydric acid. while stirring, then at 160 ~ 200 DEG C in a kettle.
React 18 ~ 24 hours;
(4) by the product of step (3) gained, after ultra-pure water and dehydrated alcohol centrifuge washing three times, at 50 DEG C, vacuum is done
Dry, i.e. prepare Co-TiO2/MoS2;
Described n-butyllithium solution is the hexane solution of n-BuLi, and concentration is 1.6 mol/L;
Described cobalt salt is selected from one of following: cobaltous sulfate, cobaltous chloride, cobalt nitrate, cobalt acetate, organic cobalt compounds;
Described non-polar solven is selected from one of following: hexane, hexamethylene, carbon tetrachloride, benzene, toluene;
Described water bath sonicator processes, and the process time is 1 hour;
Step b prepares concretely comprising the following steps of parathion sensor:
(1) with ITO electro-conductive glass as working electrode, at the Co-TiO of electrode surface drop coating 8 ~ 12 L2/MoS2Colloidal sol, under room temperature
Dry;
(2) the electrode buffer solution PBS that will obtain in step (1), continues at electrode surface drop coating 8 ~ 12 L 10
The parathion antibody-solutions of g/mL, preserves in 4 DEG C of refrigerators and dries;
(3) the electrode PBS that will obtain in step (2), continuing in electrode surface drop coating 8 ~ 12 L concentration is 100 g/
The bovine serum albumin solution of mL, preserves in 4 DEG C of refrigerators and dries;
(4) the electrode PBS that will obtain in step (3), preserves after drying in 4 DEG C of refrigerators, i.e. prepares parathion and passes
Sensor;
Described Co-TiO2/MoS2Colloidal sol is by the Co-TiO of 50 mg2/MoS2Powder is dissolved in 10 mL ultra-pure waters, and ultrasonic
The hydrosol prepared after 30 min;
Described PBS is the phosphate buffered solution of 10 mmol/L, and the pH value of described phosphate buffered solution is 7.4.
The application of the parathion sensor prepared by preparation method the most of the present invention, it is characterised in that include as follows
Applying step:
A. standard solution preparation: prepare the parathion standard solution of one group of variable concentrations including blank standard specimen;
B. working electrode modify: by the parathion sensor prepared by preparation method as claimed in claim 1 be work electricity
Pole, by the parathion standard solution of the variable concentrations of preparation in step a, drop coating is to working electrode surface respectively, in 4 DEG C of refrigerators
Preserve;
C. working curve is drawn:, repaiied with step b as reference electrode, platinum electrode as to electrode by Ag/AgCl electrode
The working electrode composition three-electrode system adornd, is connected on electrochemiluminescdetection detection equipment;Successively add in a cell
The K of 15 mL2S2O8Solution and the H of 100 L2O2Solution;Cyclical voltage is applied with the cyclic voltammetry working electrode to assembling;
Relation between light signal strength and the parathion antigen concentration of standard solution of the electrogenerated chemiluminescence according to gained, drawing
Curve;The light signal strength of blank standard specimen is designated asD 0, the light signal strength of the parathion standard solution containing variable concentrations is designated asD i, the difference that response light signal intensity reduces is ΔD = D 0-D i, ΔDMass concentration with parathion standard solutionCBetween become
Linear relationship, draws ΔD-CWorking curve;
D. the detection of parathion: replace the parathion standard solution in step a with testing sample, according to the side in step b and c
Method detects, the difference DELTA reduced according to response light signal intensityDAnd working curve, obtain containing of parathion in testing sample
Amount;
Described K2S2O8Solution is by 1 mol K2S2O8It is dissolved in the pH=6.5 buffer solution of 10 L with 1 mol KCl and being prepared into
Arrive, described pH=6.5 buffer solution be pH value be the phosphate buffered solution of 6.5;
Described H2O2Solution is aqueous hydrogen peroxide solution, and the concentration of described aqueous hydrogen peroxide solution is 10%.
The useful achievement of the present invention
(1) parathion sensor of the present invention preparation is simple, easy to operate, it is achieved that quick, sensitive, high to parathion
Selective enumeration method, and low cost, can be applicable to portable inspectiont, has market development prospect;
(2) present invention uses the method for In-situ reaction to be prepared for novel photocatalyst Co-TiO first2/MoS2, the method is main
There are three advantages: one is, due to cobalt growth in situ on nano titania square fully and nano titania square
Contact, utilizes the metal surface plasma body effect of cobalt, is effectively increased semiconductor substrate Resonance energy transfer ability, solves
Although titanium dioxide nanoplate specific surface area is bigger and mesoporous characteristic is applicable to electrogenerated chemiluminescence host material, but electroluminescent
The technical problem that chemiluminescence signal is unstable;Two are, due to the load characteristic and two of molybdenum bisuphide lamellar two-dimension nano materials
TiOx nano square thereon fully dispersed, greatly increases electrogenerated chemiluminescence intensity, solves titanium dioxide and receive
Rice sheet poorly conductive and electrogenerated chemiluminescence intensity are weak and be unfavorable for preparing the technical problem of Electrochemiluminescsensor sensor;Three
It is, due to cobalt ion the most not only as intercalation material but also as reaction dopant material, finally to use the side of In-situ reaction
Method achieves one pot of preparation of this composite, not only saves time, spillage of material, and makes the two of the cobalt doped of preparation
TiOx nano square can preferably evenly spread to above molybdenum bisuphide lamellar two-dimension nano materials.Therefore, this material
Effectively preparation, has important scientific meaning and using value;
(3) present invention is first by Co-TiO2/MoS2It is applied in the preparation of electroluminescent chemiluminescence biosensor, significantly improves
The strength and stability of electrogenerated chemiluminescence, substantially increases the detection sensitivity of Electrochemiluminescsensor sensor so that electricity
Cause chemiluminescence biosensor and achieve the application in real work;The application of this material, is also associated biomolecule sensor,
Provide Technical Reference such as Optical Electro-Chemistry sensor, electrochemical sensor etc., there is the most potential use value.
Detailed description of the invention
Embodiment 1 Co-TiO2/MoS2Preparation
(1) take 0.6 g molybdenum disulfide powder and 0.2 mmol cobalt salt joins in 3mL n-butyllithium solution jointly, protect at nitrogen
Protect with at 60 DEG C, stir 12 hours, obtain reacted solution;
(2) utilize reacted solution in non-polar solven washing step (1), at 60 DEG C, then carry out water bath sonicator process,
After having processed, the solution after recycling non-polar solven carrying out washing treatment, vacuum drying, obtain the molybdenum disulfide nano material of cobalt intercalation
Material;
(3) the molybdenum disulfide nano material taking the cobalt intercalation that 500 mg steps (2) prepare joins in 5 mL butyl titanates, stirs
After mixing 1 hour, it is slowly added to 0.5 mL Fluohydric acid. while stirring, then reacts 18 hours in a kettle. at 160 DEG C;
(4) by the product of step (3) gained, after ultra-pure water and dehydrated alcohol centrifuge washing three times, at 50 DEG C, vacuum is done
Dry, i.e. prepare Co-TiO2/MoS2;
Described n-butyllithium solution is the hexane solution of n-BuLi, and concentration is 1.6 mol/L;
Described cobalt salt is cobaltous sulfate;
Described non-polar solven is hexane;
Described water bath sonicator processes, and the process time is 1 hour.
Embodiment 2 Co-TiO2/MoS2Preparation
(1) take 0.6 g molybdenum disulfide powder and 1.0 mmol cobalt salts join in 5 mL n-butyllithium solutions jointly, protect at nitrogen
Protect with at 30 DEG C, stir 24 hours, obtain reacted solution;
(2) utilize reacted solution in non-polar solven washing step (1), at 30 DEG C, then carry out water bath sonicator process,
After having processed, the solution after recycling non-polar solven carrying out washing treatment, vacuum drying, obtain the molybdenum disulfide nano material of cobalt intercalation
Material;
(3) the molybdenum disulfide nano material taking the cobalt intercalation that 200 mg steps (2) prepare joins in 5 mL butyl titanates, stirs
After mixing 1 hour, it is slowly added to 0.6 mL Fluohydric acid. while stirring, then reacts 20 hours in a kettle. at 180 DEG C;
(4) by the product of step (3) gained, after ultra-pure water and dehydrated alcohol centrifuge washing three times, at 50 DEG C, vacuum is done
Dry, i.e. prepare Co-TiO2/MoS2;
Described n-butyllithium solution is the hexane solution of n-BuLi, and concentration is 1.6 mol/L;
Described cobalt salt is cobaltous chloride;
Described non-polar solven is carbon tetrachloride;
Described water bath sonicator processes, and the process time is 1 hour.
Embodiment 3 Co-TiO2/MoS2Preparation
(1) take 0.6 g molybdenum disulfide powder and 2.0 mmol cobalt salts join in 10 mL n-butyllithium solutions, at nitrogen jointly
Protection, with at 50 DEG C, is stirred 48 hours, is obtained reacted solution;
(2) utilize reacted solution in non-polar solven washing step (1), at 50 DEG C, then carry out water bath sonicator process,
After having processed, the solution after recycling non-polar solven carrying out washing treatment, vacuum drying, obtain the molybdenum disulfide nano material of cobalt intercalation
Material;
(3) the molybdenum disulfide nano material taking the cobalt intercalation that 10 mg steps (2) prepare joins in 5 mL butyl titanates, stirs
After mixing 1 hour, it is slowly added to 0.8 mL Fluohydric acid. while stirring, then reacts 24 hours in a kettle. at 200 DEG C;
(4) by the product of step (3) gained, after ultra-pure water and dehydrated alcohol centrifuge washing three times, at 50 DEG C, vacuum is done
Dry, i.e. prepare Co-TiO2/MoS2;
Described n-butyllithium solution is the hexane solution of n-BuLi, and concentration is 1.6 mol/L;
Described cobalt salt is cobalt acetate;
Described non-polar solven is benzene;
Described water bath sonicator processes, and the process time is 1 hour.
The preparation method of embodiment 4 parathion sensor
(1) using a width of 1 cm, a length of 4 cm ITO electro-conductive glass as working electrode, at the Co-of electrode surface drop coating 8 L
TiO2/MoS2Colloidal sol, dries under room temperature;
(2) the electrode buffer solution PBS that will obtain in step (1), continues at electrode surface drop coating 8 L 10 g/mL
Parathion antibody-solutions, 4 DEG C of refrigerators preserve and dry;
(3) the electrode PBS that will obtain in step (2), continuing in electrode surface drop coating 8 L concentration is 100 g/mL
Bovine serum albumin solution, 4 DEG C of refrigerators preserve and dry;
(4) the electrode PBS that will obtain in step (3), preserves in 4 DEG C of refrigerators after drying, and i.e. prepares parathion sensing
Device;
Described Co-TiO2/MoS2Colloidal sol is by the Co-TiO of 50 mg2/MoS2Powder is dissolved in 10 mL ultra-pure waters, and ultrasonic
The hydrosol prepared after 30 min;
Described PBS is the phosphate buffered solution of 10mmol/L, and the pH value of described phosphate buffered solution is 7.4.
The preparation method of embodiment 5 parathion sensor
(1) using a width of 1 cm, a length of 4 cm ITO electro-conductive glass as working electrode, at the Co-of electrode surface drop coating 10 L
TiO2/MoS2Colloidal sol, dries under room temperature;
(2) the electrode buffer solution PBS that will obtain in step (1), continues at electrode surface drop coating 10 L 10 g/
The parathion antibody-solutions of mL, preserves in 4 DEG C of refrigerators and dries;
(3) the electrode PBS that will obtain in step (2), continuing in electrode surface drop coating 10 L concentration is 100 g/mL
Bovine serum albumin solution, 4 DEG C of refrigerators preserve and dry;
(4) the electrode PBS that will obtain in step (3), preserves after drying in 4 DEG C of refrigerators, i.e. prepares parathion and passes
Sensor;
Described Co-TiO2/MoS2Colloidal sol is by the Co-TiO of 50 mg2/MoS2Powder is dissolved in 10 mL ultra-pure waters, and ultrasonic
The hydrosol prepared after 30 min;
Described PBS is the phosphate buffered solution of 10 mmol/L, and the pH value of described phosphate buffered solution is 7.4.
The preparation method of embodiment 6 parathion sensor
(1) using a width of 1 cm, a length of 4 cm ITO electro-conductive glass as working electrode, at the Co-of electrode surface drop coating 12 L
TiO2/MoS2Colloidal sol, dries under room temperature;
(2) the electrode buffer solution PBS that will obtain in step (1), continues at electrode surface drop coating 12 L 10 g/
The parathion antibody-solutions of mL, preserves in 4 DEG C of refrigerators and dries;
(3) the electrode PBS that will obtain in step (2), continuing in electrode surface drop coating 12 L concentration is 100 g/mL
Bovine serum albumin solution, 4 DEG C of refrigerators preserve and dry;
(4) the electrode PBS that will obtain in step (3), preserves after drying in 4 DEG C of refrigerators, i.e. prepares parathion and passes
Sensor;
Described Co-TiO2/MoS2Colloidal sol is by the Co-TiO of 50 mg2/MoS2Powder is dissolved in 10 mL ultra-pure waters, and ultrasonic
The hydrosol prepared after 30 min;
Described PBS is the phosphate buffered solution of 10 mmol/L, and the pH value of described phosphate buffered solution is 7.4.
The parathion sensor of embodiment 7 embodiment 1 ~ 6 preparation, is applied to the detection of parathion, and step is as follows:
(1) standard solution preparation: prepare the parathion standard solution of one group of variable concentrations including blank standard specimen;
(2) working electrode modify: by the parathion sensor prepared by preparation method as claimed in claim 1 be work electricity
Pole, by the drop coating respectively of the parathion standard solution of the variable concentrations of preparation in step (1) to working electrode surface, 4 DEG C of refrigerators
Middle preservation;
(3) working curve is drawn: using saturated calomel electrode as reference electrode, platinum electrode is as auxiliary electrode, with step (2)
The working electrode composition three-electrode system modified, is connected on electrochemiluminescdetection detection equipment;In a cell successively
Add the K of 15 mL2S2O8Solution and the H of 100 L2O2Solution;Circulation electricity is applied with the cyclic voltammetry working electrode to assembling
Pressure;Relation between light signal strength and the parathion antigen concentration of standard solution of the electrogenerated chemiluminescence according to gained, draws
Working curve;The light signal strength of blank standard specimen is designated asD 0, the light signal strength of the parathion standard solution containing variable concentrations
It is designated asD i, the difference that response light signal intensity reduces is ΔD = D 0-D i, ΔDMass concentration with parathion standard solutionCIt
Between linear, draw ΔD-CWorking curve;The linear detection range of parathion is: 0.003 ~ 100 ng/mL, detection limit
For: 1.1 pg/mL;
(4) detection of parathion: replace the parathion standard solution in step a with testing sample, according to the side in step b and c
Method detects, the difference DELTA reduced according to response light signal intensityDAnd working curve, obtain containing of parathion in testing sample
Amount;
Described K2S2O8Solution is by 1 mol K2S2O8It is dissolved in the pH=6.5 buffer solution of 10 L with 1 mol KCl and being prepared into
Arrive, described pH=6.5 buffer solution be pH value be the phosphate buffered solution of 6.5;
Described H2O2Solution is aqueous hydrogen peroxide solution, and the concentration of described aqueous hydrogen peroxide solution is 10%.
Claims (4)
1. the preparation method of the parathion sensor built based on two-dimension nano materials, it is characterised in that described parathion
Sensor is made up of working electrode, two-dimension nano materials, parathion antibody, bovine serum albumin;Described two-dimension nano materials
Two-dimensional nano composite Co-TiO for cobalt doped nano titania square In-situ reaction molybdenum bisuphide2/MoS2。
2. the preparation method of the parathion sensor built based on two-dimension nano materials as claimed in claim 1, its feature exists
Following two preparation process is included in, described preparation method:
A. Co-TiO is prepared2/MoS2;
B. parathion sensor is prepared.
3. the preparation method of the parathion sensor built based on two-dimension nano materials as described in claim 1 and 2, its feature
It is, described Co-TiO2/MoS2Concrete preparation process be:
(1) take 0.6 g molybdenum disulfide powder and 0.2 ~ 2.0 mmol cobalt salt joins 3 ~ 10 mL n-butyllithium solutions jointly
In, at nitrogen protection and 30 ~ 60 DEG C, stir 12 ~ 48 hours, obtain reacted solution;
(2) utilize reacted solution in non-polar solven washing step (1), at 30 ~ 60 DEG C, then carry out water bath sonicator
Process, after having processed, the solution after recycling non-polar solven carrying out washing treatment, vacuum drying, obtain the molybdenum bisuphide of cobalt intercalation
Nano material;
(3) the molybdenum disulfide nano material taking the cobalt intercalation that 10 ~ 500 mg steps (2) prepare joins 5 mL butyl titanates
In, after stirring 1 hour, it is slowly added to 0.5 ~ 0.8 mL Fluohydric acid. while stirring, then at 160 ~ 200 DEG C in a kettle.
React 18 ~ 24 hours;
(4) by the product of step (3) gained, after ultra-pure water and dehydrated alcohol centrifuge washing three times, at 50 DEG C, vacuum is done
Dry, i.e. prepare Co-TiO2/MoS2;
Described n-butyllithium solution is the hexane solution of n-BuLi, and concentration is 1.6 mol/L;
Described cobalt salt is selected from one of following: cobaltous sulfate, cobaltous chloride, cobalt nitrate, cobalt acetate, organic cobalt compounds;
Described non-polar solven is selected from one of following: hexane, hexamethylene, carbon tetrachloride, benzene, toluene;
Described water bath sonicator processes, and the process time is 1 hour.
4. the preparation method of the parathion sensor built based on two-dimension nano materials as described in claim 1 and 2, its feature
Being, the concrete preparation process of described parathion sensor is:
(1) with ITO electro-conductive glass as working electrode, at the Co-TiO of electrode surface drop coating 8 ~ 12 L2/MoS2Colloidal sol, under room temperature
Dry;
(2) the electrode buffer solution PBS that will obtain in step (1), continues at electrode surface drop coating 8 ~ 12 L 10
The parathion antibody-solutions of g/mL, preserves in 4 DEG C of refrigerators and dries;
(3) the electrode PBS that will obtain in step (2), continuing in electrode surface drop coating 8 ~ 12 L concentration is 100 g/
The bovine serum albumin solution of mL, preserves in 4 DEG C of refrigerators and dries;
(4) the electrode PBS that will obtain in step (3), preserves after drying in 4 DEG C of refrigerators, i.e. prepares parathion and passes
Sensor;
Described Co-TiO2/MoS2Colloidal sol is by the Co-TiO of 50 mg2/MoS2Powder is dissolved in 10 mL ultra-pure waters, and ultrasonic
The hydrosol prepared after 30 min;
Described PBS is the phosphate buffered solution of 10 mmol/L, and the pH value of described phosphate buffered solution is 7.4.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610521134.7A CN106198657B (en) | 2016-07-05 | 2016-07-05 | A kind of preparation method of the parathion sensor based on two-dimension nano materials building |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610521134.7A CN106198657B (en) | 2016-07-05 | 2016-07-05 | A kind of preparation method of the parathion sensor based on two-dimension nano materials building |
Publications (2)
Publication Number | Publication Date |
---|---|
CN106198657A true CN106198657A (en) | 2016-12-07 |
CN106198657B CN106198657B (en) | 2019-03-12 |
Family
ID=57465097
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201610521134.7A Expired - Fee Related CN106198657B (en) | 2016-07-05 | 2016-07-05 | A kind of preparation method of the parathion sensor based on two-dimension nano materials building |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN106198657B (en) |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20060239907A1 (en) * | 2003-06-03 | 2006-10-26 | The Trustees Of The University Of Pennsylvania | Stealthy nano agents |
CN103913565A (en) * | 2014-04-26 | 2014-07-09 | 济南大学 | Preparation method and application of immunosensor constructed by difunctional marker |
CN105572193A (en) * | 2016-02-25 | 2016-05-11 | 王亚莉 | Preparation method and application of electrochemical chlordimeform sensor based on composite cerium-doped porous nanocomposite |
CN105675689A (en) * | 2016-03-16 | 2016-06-15 | 济南大学 | Preparation method for hydrogen peroxide non-enzymatic sensor established based on molybdenum sulfide composite and application |
CN105717181A (en) * | 2016-02-25 | 2016-06-29 | 济南大学 | Preparation method and application of electrochemical malathion biosensor based on bi-metal in-situ composite two-dimensional nanomaterial |
-
2016
- 2016-07-05 CN CN201610521134.7A patent/CN106198657B/en not_active Expired - Fee Related
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20060239907A1 (en) * | 2003-06-03 | 2006-10-26 | The Trustees Of The University Of Pennsylvania | Stealthy nano agents |
CN103913565A (en) * | 2014-04-26 | 2014-07-09 | 济南大学 | Preparation method and application of immunosensor constructed by difunctional marker |
CN105572193A (en) * | 2016-02-25 | 2016-05-11 | 王亚莉 | Preparation method and application of electrochemical chlordimeform sensor based on composite cerium-doped porous nanocomposite |
CN105717181A (en) * | 2016-02-25 | 2016-06-29 | 济南大学 | Preparation method and application of electrochemical malathion biosensor based on bi-metal in-situ composite two-dimensional nanomaterial |
CN105675689A (en) * | 2016-03-16 | 2016-06-15 | 济南大学 | Preparation method for hydrogen peroxide non-enzymatic sensor established based on molybdenum sulfide composite and application |
Non-Patent Citations (2)
Title |
---|
KE-JING HUANG等: "Amperometric immunobiosensor for α-fetoprotein using Au nanoparticles/chitosan/TiO2–graphene composite based platform", 《BIOELECTROCHEMISTRY》 * |
LINGXIA ZHENG等: "Hierarchical MoS2 Nanosheet@TiO2 Nanotube Array Composites with Enhanced Photocatalytic and Photocurrent Performances", 《SMALL》 * |
Also Published As
Publication number | Publication date |
---|---|
CN106198657B (en) | 2019-03-12 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN105628758B (en) | A kind of preparation method and application of the optical electro-chemistry parathion sensor based on two-dimensional nano light-sensitive material | |
CN105717180B (en) | A kind of preparation method and application of the optical electro-chemistry aflatoxin biology sensor based on two-dimensional nano composite | |
CN105717181A (en) | Preparation method and application of electrochemical malathion biosensor based on bi-metal in-situ composite two-dimensional nanomaterial | |
CN106198501B (en) | A kind of preparation method for the Electrochemiluminescsensor sensor detecting aflatoxin | |
CN105572193A (en) | Preparation method and application of electrochemical chlordimeform sensor based on composite cerium-doped porous nanocomposite | |
CN105738437B (en) | A kind of preparation method and application of the electrochemistry parathion sensor based on metal and metal oxide co-doped nano composite | |
CN105572108B (en) | A kind of preparation method and application of electrogenerated chemiluminescence demeton sensor | |
CN105699645A (en) | Application and preparation method of electrochemical salbutamol sensor | |
CN106124588B (en) | A kind of preparation method of the electrochemistry nonyl phenol sensor based on titania-doped/molybdenum disulfide composite material | |
CN105675685A (en) | Preparation method and application of electrochemical chlordimeform sensor based on manganese-doped two-dimensional nano composite material | |
CN105717178A (en) | Preparation method and application of electrochemical diethylstilbestrol sensor based on titanium-dioxide-based two-dimensional composite nanomaterial | |
CN105738353B (en) | A kind of preparation method and application of optical electro-chemistry decis sensor | |
CN106124591B (en) | A kind of preparation method based on titanium dioxide/molybdenum disulfide composite material estradiol sensor | |
CN106198682B (en) | A kind of preparation method of the optical electro-chemistry furazolidone sensor based on bimetallic codope two-dimensional light sensitive agent | |
CN106053572B (en) | A kind of preparation method of electrochemistry bisphenol-A sensor | |
CN106124589B (en) | A kind of preparation method of the electrochemica biological sensor based on the building of Fe2O3 doping two-dimension nano materials | |
CN105717099B (en) | A kind of preparation method and application of electrogenerated chemiluminescence furazolidone biology sensor | |
CN106053442B (en) | A kind of preparation method of the electrogenerated chemiluminescence decis sensor based on iron cobalt codope two-dimension nano materials | |
CN106198683B (en) | A kind of preparation method of the optical electro-chemistry chloramphenicol biosensor based on two-dimensional nano photoelectric material | |
CN106198657A (en) | A kind of preparation method of the parathion sensor built based on two-dimension nano materials | |
CN106198672B (en) | A kind of preparation method for the electrochemical sensor detecting carbamate | |
CN106198668B (en) | A kind of preparation method of the optical electro-chemistry demeton sensor based on cobalt doped two-dimensional nano photoelectric material | |
CN105738350A (en) | Preparing method and application of electrochemiluminescence carbamate sensor based on cobalt-doped two-dimensional nanometer composite | |
CN106248753B (en) | A kind of preparation method of the optical electro-chemistry Spanon sensor based on load type double-metal codope photosensitizer | |
CN106198500B (en) | A kind of preparation method for the electroluminescent chemiluminescence biosensor detecting organo-chlorine pesticide |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190312 Termination date: 20210705 |