CN106053566A - Preparation method of photoelectrochemical salbutamol sensor based on two-dimensional magnetic nano photoelectric material - Google Patents
Preparation method of photoelectrochemical salbutamol sensor based on two-dimensional magnetic nano photoelectric material Download PDFInfo
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Abstract
The invention discloses a preparation method of a photoelectrochemical salbutamol sensor and belongs to the technical field of novel nano functional materials and biosensors. The preparation method includes: preparing a novel two-dimensional magnetic nano photoelectric material, namely a two-dimensional nano composite material Fe-TiO2/MoS2 with an iron-doped titanium dioxide nano square block composited with molybdenum disulfide in situ; utilizing high biocompatibility and large specific surface of the material to load a salbutamol antibody and fix alkaline phosphatase; during detection, due to the fact that alkaline phosphatase can catalyze L-ascorbic acid-2-trisodium phosphate AAP to generate L-ascorbic acid in situ so as to provide an electron donor for photoelectric detection, utilizing influence of specific quantitative combining of the antibody and antigen on electron transmission capability to correspondingly lower photoelectric current strength; finally realizing construction of the photoelectric sensor adopting a mark-free photoelectrochemical method to detect salbutamol.
Description
Technical field
The present invention relates to the preparation method of a kind of Optical Electro-Chemistry albuterol sensor.Belong to Nano-function thin films with
Biosensor technology field.
Background technology
Albuterol is selectivity beta 2 receptor agonist, is used as clenbuterol hydrochloride, improves live pig in modern Carnis Sus domestica cultivation
Lean meat yield.Within 2002, begin, be listed in cultivation industry forbidden drug, must not add in livestock and poultry cultivation.
At present, the method for detection albuterol mainly has chromatography, mass spectrography etc..This type of method instrument is valuable, operation is multiple
Miscellaneous, laboratory personnel just can detect after needing professional training.Therefore, R&D costs are low, detect fast, highly sensitive, specificity
Strong albuterol sensor is significant.
Optical Electro-Chemistry sensor is due to the feature such as highly sensitive, testing cost is low, in recent years by increasing researcher
Paid close attention to.Optical Electro-Chemistry sensor is to cause electron-hole pair to separate based on additional light source activation Electrophotosensitivmaterial material,
The most partially under potential condition, it is achieved the electronics quick transmission on electrode, quasiconductor and trim and analyte, and form light
Electric current.In optimal conditions, the change of analyte concentration can directly affect the size of photoelectric current, and recycling biological immune combines,
Just can realize the qualitative and quantitative analysis to analyte according to the change of photoelectric current.
Optical Electro-Chemistry sensor most critical technology is exactly the raising of the performances such as the size to photoelectric current and stability.Titanium dioxide
Titanium is a kind of photocatalyst and light induced electron host material being most widely used, but, the reality of titanium dioxide to be given full play to
Border application level, needs one side to improve Optical Electro-Chemistry work by regulating and controlling its material morphology to expose more high activity crystal faces
Property, on the other hand improve the sun by doping different metal or metal-oxide regulation and control photosensitive wavelength to visible-range extension
The utilization rate of light.Due to two dimension titanium dioxide nano material, such as titanium dioxide nanoplate, nano titania square etc., it is possible to
Exposing more high activity crystal face, have higher Optical Electro-Chemistry activity, titanium dioxide nanoplate has more preferable than nanoparticle
Ground application prospect, the research for titanium dioxide nanoplate also receives much concern.And single titanium dioxide nano material is photosensitive
Wavelength is typically in ultra-violet (UV) band, and interacts due to bad dispersibility, easily stacking, thus reduces Optical Electro-Chemistry activity, unfavorable
Apply in reality.Therefore, R&D costs are low, photosensitive dose active of titanium dioxide has important to prepare simple high Optical Electro-Chemistry
Scientific meaning and using value.
(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, have before the photosensitizer of excellent photoelectrochemical behaviour has a wide range of applications for In-situ reaction preparation
Scape and important scientific meaning.
Additionally, the photo-generate electron-hole of single titanium dioxide nano material is to the most compound, thus cause photosignal
Weaken, and titanium dioxide poorly conductive also limit the Optical Electro-Chemistry sensor that built by single titanium dioxide nano material
Sensitivity is the highest, is unfavorable for actual application.Therefore, design, prepare efficient, stable doping titanium dioxide nano sheet and
Trim is the key technology preparing Optical Electro-Chemistry sensor.
Summary of the invention
It is an object of the invention to provide a kind of prepare simple, highly sensitive, detection quickly, the Optical Electro-Chemistry of high specificity
The preparation method of albuterol sensor, prepared sensor, can be used for quick, the Sensitive Detection of albuterol.Based on this
Purpose, the method comprises the steps of firstly, preparing a kind of New Two Dimensional magnetic Nano photoelectric material, i.e. Fe2O3 doping nano titania square is former
The two-dimensional nano composite Fe-TiO of position composite molybdenum disulfide2/MoS2, utilize the good biocompatibility of this material with big
Specific surface area, albuterol antibody in load, fixing upper alkali phosphatase, when detecting, owing to alkali phosphatase can
Produce L-AA AA in situ with catalysis L-AA-2-tricresyl phosphate sodium salt AAP, and and then provide electronics for Photoelectric Detection
Donor, recycling antibody is combined the impact on electron transport ability with the specific quantification of antigen so that photo-current intensity is corresponding
Reduce, finally achieve the structure of the photoelectric sensor using unmarked PhotoelectrochemicalMethod Method detection albuterol.
The technical solution used in the present invention is as follows:
1. a preparation method for Optical Electro-Chemistry albuterol sensor based on two-dimensional magnetic nanometer photoelectronic material, its feature
It is the two dimension that described two-dimensional magnetic nanometer photoelectronic material is Fe2O3 doping nano titania square In-situ reaction molybdenum bisuphide
Nano composite material Fe-TiO2/MoS2, described Optical Electro-Chemistry albuterol sensor is by working electrode, Fe-TiO2/MoS2、
Albuterol antibody, alkali phosphatase, bovine serum albumin form；
It is characterized in that, described preparation method includes following preparation process:
A. Fe-TiO is prepared2/MoS2；
B. Optical Electro-Chemistry albuterol sensor is prepared；
Wherein, step a prepares Fe-TiO2/MoS2Concretely comprise the following steps:
(1) take 0.6 g molybdenum disulfide powder and 0.2 ~ 2.0 mmol iron 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 ferrum intercalation
Nano material；
(3) the molybdenum disulfide nano material taking the ferrum 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 Fe-TiO2/MoS2；
Described n-butyllithium solution is the hexane solution of n-BuLi, and concentration is 1.6 mol/L；
Described iron salt is selected from one of following: iron sulfate, iron chloride, ferric nitrate, ferric acetate, organoiron compound；
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 Optical Electro-Chemistry albuterol sensor:
(1) with ITO electro-conductive glass as working electrode, at the Fe-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 albuterol 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 6 ~ 10 L concentration is 20 g/
The alkaline phosphatase enzymatic solution of mL, preserves in 4 DEG C of refrigerators and dries；
(4) the electrode PBS that will obtain in step (3), 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；
(5) the electrode PBS that will obtain in step (4), preserves in 4 DEG C of refrigerators after drying, i.e. prepares Optical Electro-Chemistry
Albuterol sensor；
Described Fe-TiO2/MoS2Colloidal sol is by the Fe-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 Optical Electro-Chemistry albuterol sensor prepared by preparation method the most of the present invention, its feature exists
In, including following applying step:
A. standard solution preparation: prepare the albuterol standard solution of one group of variable concentrations including blank standard specimen；
B. working electrode is modified: by the Optical Electro-Chemistry albuterol sensor prepared by preparation method as claimed in claim 1
For working electrode, by the drop coating respectively of the albuterol standard solution of the variable concentrations of preparation in step b to working electrode surface, 4
DEG C refrigerator preserves；
C. working curve is drawn: using saturated calomel electrode as reference electrode, platinum electrode is as auxiliary electrode, with step b institute
The working electrode composition three-electrode system modified, is connected on Optical Electro-Chemistry detection equipment；Successively add in a cell
The Tris HCl buffer solution of 15mL pH=9.6 and the L-AA-2-tricresyl phosphate sodium salt AAP of 5 mL 10 mmol/L are molten
Liquid；Use i-t means of testing, according to the relation between photocurrent values and the albuterol concentration of standard solution of gained, draw work
Make curve；
D. the detection of albuterol: replace the albuterol standard solution in step a with testing sample, according in step b and c
Method detect, according to the response intensity level of signal and working curve, obtain the content of albuterol in testing sample.
The useful achievement of the present invention
(1) Optical Electro-Chemistry albuterol sensor of the present invention preparation is simple, easy to operate, it is achieved that fast to sample
Selective enumeration method fast, sensitive, high, 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 Fe-TiO first2/MoS2, the method is main
There are three advantages: one is, due to ferrum growth in situ on nano titania square fully and nano titania square
Contact, utilizes the metal surface plasma body effect of ferrum, effectively prevents photo-generate electron-hole to being combined, be greatly enhanced
Photocatalytic activity, due to the effect of metal ion, has widened photosensitive wavelength ground scope, it is achieved that in visible region ground photocatalysis
Effect, drastically increases sunlight ground utilization ratio, although it is good to solve two dimension titanium dioxide nano material photocatalysis effect,
But the technical problem of photocatalysis effect difference under sunlight；Two are, due to molybdenum bisuphide lamellar two-dimension nano materials
Load characteristic and nano titania square thereon fully dispersed, the light greatly increasing nano titania square is urged
With solving two dimension titanium dioxide nano material, change activity is unfavorable for that dispersion reduces the technical problem of photocatalytic activity；Three are,
Due to iron ion the most not only as intercalation material but also as reaction dopant material, the method finally using In-situ reaction is real
Show one pot of preparation of this composite, not only saved time, spillage of material, and make the titanium dioxide of the Fe2O3 doping of preparation
Titanium nano square can preferably evenly spread to above molybdenum bisuphide lamellar two-dimension nano materials.Therefore, this material is effective
Preparation, has important scientific meaning and using value；
(3) present invention is first by Fe-TiO2/MoS2It is applied in the preparation of Photoelectrochemistrbiosensor biosensor, significantly improves light
The valid density of raw carrier, substantially increases the detection sensitivity of Optical Electro-Chemistry sensor so that Optical Electro-Chemistry bio-sensing
Device achieves the application in real work；The application of this material, is also associated biomolecule sensor, as electrogenerated chemiluminescence senses
Device, electrochemical sensor etc. provide Technical Reference, have the most potential use value.
Detailed description of the invention
Embodiment 1 Fe-TiO2/MoS2Preparation
(1) take 0.6 g molybdenum disulfide powder and 0.2 mmol iron 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 ferrum intercalation
Material；
(3) the molybdenum disulfide nano material taking the ferrum 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 Fe-TiO2/MoS2；
Described n-butyllithium solution is the hexane solution of n-BuLi, and concentration is 1.6 mol/L；
Described iron salt is iron sulfate；
Described non-polar solven is hexane；
Described water bath sonicator processes, and the process time is 1 hour.
Embodiment 2 Fe-TiO2/MoS2Preparation
(1) take 0.6 g molybdenum disulfide powder and 1.0 mmol iron salt 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 ferrum intercalation
Material；
(3) the molybdenum disulfide nano material taking the ferrum 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 Fe-TiO2/MoS2；
Described n-butyllithium solution is the hexane solution of n-BuLi, and concentration is 1.6 mol/L；
Described iron salt is iron chloride；
Described non-polar solven is carbon tetrachloride；
Described water bath sonicator processes, and the process time is 1 hour.
Embodiment 3 Fe-TiO2/MoS2Preparation
(1) take 0.6 g molybdenum disulfide powder and 2.0 mmol iron salt 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 ferrum intercalation
Material；
(3) the molybdenum disulfide nano material taking the ferrum 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 Fe-TiO2/MoS2；
Described n-butyllithium solution is the hexane solution of n-BuLi, and concentration is 1.6 mol/L；
Described iron salt is ferric 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 Optical Electro-Chemistry albuterol sensor
(1) using a width of 1 cm, a length of 4 cm ITO electro-conductive glass as working electrode, at the Fe-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
Albuterol 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), continuing in electrode surface drop coating 6 L concentration is 20 g/mL's
Alkaline phosphatase enzymatic solution, preserves in 4 DEG C of refrigerators and dries；
(5) the electrode PBS that will obtain in step (4), preserves in 4 DEG C of refrigerators after drying, i.e. prepares Optical Electro-Chemistry
Albuterol sensor；
Described Fe-TiO2/MoS2Colloidal sol is by the Fe-TiO prepared by the embodiment 1 of 50 mg2/MoS2Powder is dissolved in 10 mL
In ultra-pure water, and the hydrosol prepared after ultrasonic 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 Optical Electro-Chemistry albuterol sensor
All preparation processes are with embodiment 4, the Fe-TiO of a middle use2/MoS2For the Fe-prepared by embodiment 2
TiO2/MoS2。
The preparation method of embodiment 6 Optical Electro-Chemistry albuterol sensor
All preparation processes are with embodiment 4, the Fe-TiO of a middle use2/MoS2For the Fe-prepared by embodiment 3
TiO2/MoS2。
The Optical Electro-Chemistry albuterol sensor of embodiment 7 embodiment 1 and 3 preparation, is applied to the detection of albuterol,
Step is as follows:
(1) standard solution preparation: prepare the albuterol standard solution of one group of variable concentrations including blank standard specimen；
(2) working electrode is modified: by the Optical Electro-Chemistry albuterol sensor prepared by preparation method as claimed in claim 1
For working electrode, by the drop coating respectively of the albuterol standard solution of the variable concentrations of preparation in step (1) to working electrode surface,
4 DEG C of refrigerators preserve；
(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 Optical Electro-Chemistry detection equipment；Successively add in a cell
The Tris HCl buffer solution of 15mL pH=9.6 and the L-AA-2-tricresyl phosphate sodium salt AAP of 5 mL 10 mmol/L are molten
Liquid；Use i-t means of testing, according to the relation between photocurrent values and the albuterol concentration of standard solution of gained, draw work
Make curve；The linear detection range of albuterol is: 0.002 ~ 200 ng/mL, and detection is limited to: 0.8 pg/mL；
(4) actual sample detection: replace the albuterol standard solution in step (1) with testing sample, according to step (2) and
(3) method in detects, and according to the response intensity level of signal and working curve, obtains containing of albuterol in testing sample
Amount.
The Optical Electro-Chemistry albuterol sensor of embodiment 8 embodiment 2 and 4 preparation, is applied to the detection of albuterol,
Step is as follows:
(1) standard solution preparation: prepare the albuterol standard solution of one group of variable concentrations including blank standard specimen；
(2) working electrode is modified: by the Optical Electro-Chemistry albuterol sensor prepared by preparation method as claimed in claim 1
For working electrode, by the drop coating respectively of the albuterol standard solution of the variable concentrations of preparation in step (1) to working electrode surface,
4 DEG C of refrigerators preserve；
(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 Optical Electro-Chemistry detection equipment；Successively add in a cell
The Tris HCl buffer solution of 15mL pH=9.6 and the L-AA-2-tricresyl phosphate sodium salt AAP of 5 mL 10 mmol/L are molten
Liquid；Use i-t means of testing, according to the relation between photocurrent values and the albuterol concentration of standard solution of gained, draw work
Make curve；The linear detection range of albuterol is: 0.002 ~ 200 ng/mL, and detection is limited to: 0.8 pg/mL；
(4) actual sample detection: replace the albuterol standard solution in step (1) with testing sample, according to step (2) and
(3) method in detects, and according to the response intensity level of signal and working curve, obtains containing of albuterol in testing sample
Amount.
The Optical Electro-Chemistry albuterol sensor of embodiment 9 embodiment 3 and 6 preparation, is applied to the detection of albuterol,
Step is as follows:
(1) standard solution preparation: prepare the albuterol standard solution of one group of variable concentrations including blank standard specimen；
(2) working electrode is modified: by the Optical Electro-Chemistry albuterol sensor prepared by preparation method as claimed in claim 1
For working electrode, by the drop coating respectively of the albuterol standard solution of the variable concentrations of preparation in step (1) to working electrode surface,
4 DEG C of refrigerators preserve；
(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 Optical Electro-Chemistry detection equipment；Successively add in a cell
The Tris HCl buffer solution of 15mL pH=9.6 and the L-AA-2-tricresyl phosphate sodium salt AAP of 5 mL 10 mmol/L are molten
Liquid；Use i-t means of testing, according to the relation between photocurrent values and the albuterol concentration of standard solution of gained, draw work
Make curve；The linear detection range of albuterol is: 0.002 ~ 200 ng/mL, and detection is limited to: 0.8 pg/mL；
(4) actual sample detection: replace the albuterol standard solution in step (1) with testing sample, according to step (2) and
(3) method in detects, and according to the response intensity level of signal and working curve, obtains containing of albuterol in testing sample
Amount.
Claims (4)
1. a preparation method for Optical Electro-Chemistry albuterol sensor based on two-dimensional magnetic nanometer photoelectronic material, its feature exists
In two wieners that described two-dimensional magnetic nanometer photoelectronic material is Fe2O3 doping nano titania square In-situ reaction molybdenum bisuphide
Nano composite material Fe-TiO2/MoS2, described Optical Electro-Chemistry albuterol sensor is by working electrode, Fe-TiO2/MoS2, husky
Butylamine alcohol antibody, alkali phosphatase, bovine serum albumin form.
2. the preparation of Optical Electro-Chemistry albuterol sensor based on two-dimensional magnetic nanometer photoelectronic material as claimed in claim 1
Method, it is characterised in that described preparation method includes following two preparation process:
A. Fe-TiO is prepared2/MoS2；
B. Optical Electro-Chemistry albuterol sensor is prepared.
3. Optical Electro-Chemistry albuterol sensor based on two-dimensional magnetic nanometer photoelectronic material as described in claim 1 and 2
Preparation method, it is characterised in that described Fe-TiO2/MoS2Concrete preparation process be:
(1) take 0.6 g molybdenum disulfide powder and 0.2 ~ 2.0 mmol iron 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 ferrum intercalation
Nano material；
(3) the molybdenum disulfide nano material taking the ferrum 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 Fe-TiO2/MoS2；
Described n-butyllithium solution is the hexane solution of n-BuLi, and concentration is 1.6 mol/L；
Described iron salt is selected from one of following: iron sulfate, iron chloride, ferric nitrate, ferric acetate, organoiron compound；
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. Optical Electro-Chemistry albuterol sensor based on two-dimensional magnetic nanometer photoelectronic material as described in claim 1 and 2
Preparation method, it is characterised in that the concrete preparation process of described Optical Electro-Chemistry albuterol sensor is:
(1) with ITO electro-conductive glass as working electrode, at the Fe-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 albuterol 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 6 ~ 10 L concentration is 20 g/
The alkaline phosphatase enzymatic solution of mL, preserves in 4 DEG C of refrigerators and dries；
(4) the electrode PBS that will obtain in step (3), 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；
(5) the electrode PBS that will obtain in step (4), preserves in 4 DEG C of refrigerators after drying, i.e. prepares Optical Electro-Chemistry
Albuterol sensor；
Described Fe-TiO2/MoS2Colloidal sol is by the Fe-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.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610521716.5A CN106053566B (en) | 2016-07-05 | 2016-07-05 | A kind of preparation method of the optical electro-chemistry salbutamol sensor based on two-dimensional magnetic nanometer photoelectronic material |
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| CN201610521716.5A CN106053566B (en) | 2016-07-05 | 2016-07-05 | A kind of preparation method of the optical electro-chemistry salbutamol sensor based on two-dimensional magnetic nanometer photoelectronic material |
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