CN107748190A - A kind of preparation method of the label-free type optical electro-chemistry sensor of zearalenone - Google Patents
A kind of preparation method of the label-free type optical electro-chemistry sensor of zearalenone Download PDFInfo
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Abstract
The present invention discloses a kind of preparation method of the label-free type optical electro-chemistry sensor of zearalenone, and the construction method of the sensing interface is to utilize Nanometer Copper ferro-cobalt material, polylysine and nano rutile-type TiO2The sight crystal that is situated between, which is used as, constructs primitive, and and then immobilization zearalenone antibody (Ab)；Due to the surface plasma effect and polylysine good electric conductivity of Nanometer Copper ferro-cobalt, the sensing interface can accelerate nano rutile-type TiO2It is situated between and sees the light induced electron transfer velocity of crystal and improve its photo-signal, while polylysine contains abundant amino, is advantageous to the load of antibody；When immune response occurs for zearalenone and the zearalenone antibody of immobilization, due to space steric effect, the photosignal of the sensing interface substantially weakens.Based on the phenomenon, it is established that label-free type photoelectric sensing method can realize to zearalenone concentration 1 × 10‑6Highly sensitive detection in the range of ng/mL -10 ng/mL.
Description
Technical field
The invention belongs to new function material and bio-sensing detection technique field, and in particular to a kind of label-free photoelectricity
Chemical sensor detects for zearalenone.
Background technology
Zearalenone (Zearalenone), also known as F-2 toxin, it is the metabolite of Gibberella zeae bacterium.It divides extensively
It is distributed in contaminated cereal and agricultural byproducts, dairy produce, especially in corn and its fabricated product.Zearalenone has
Reproductive and developmental toxicity, immunotoxicity and strong Teratogenesis toxicity etc., also can Endocrine impact, and may induce swollen
Knurl.At present, the bioassay method for detecting zearalenone mainly has EUSA, electrochemistry and fluorescence spectrum
Deng.However, the sensitivity of these methods further enhances and explored a low background signal, favorable reproducibility, wide response
The sensing platform of scope is still an urgent demand of zearalenone measure.
Optical electro-chemistry（PEC）Detection, is the one kind set up based on photoelectrochemical process and chemical/biological identification process
New analysis method.This method is using light as excitation signal, using photoelectric current as detection signal, has high sensitivity, response fast
The advantages that speed, equipment are simple and are easily miniaturized, providing one kind for fields such as clinical diagnosis, environmental monitoring and food securities has by force
Power means.Photoelectrochemical assay uses light, and as excitation signal, detection is electric signal, is made by using various forms of energy
For excitation signal and detection signal, make to excite and do not interfere with each other with detection signal, thus background signal is relatively low, can obtain higher spirit
Sensitivity.The realization of the type of photoelectric material, performance and photoelectrochemical process has direct and close relation, and photoelectric material is in itself
PhotoelectrochemicalProperties Properties, preparation method, composite effect, pattern control, charge-conduction speed etc. is for the suitable of photoelectrochemical process
Profit is realized and had a major impact.
TiO2Nano material is because of its unique photocatalytic activity, nontoxicity, excellent chemically and physically stability, make its into
For photocatalysis and the ideal material of optical electro-chemistry sensor.The performance of titanium dioxide is typically by crystal formation, grain size, crystal face, knot
The influence of brilliant degree, specific surface area, micro-structural etc..TiO2The sight crystal that is situated between is that crystal subunit ordered arrangement is formed, compared to biography
The TiO of system2Monocrystalline, TiO2The sight crystal that is situated between has more excellent solar energy conversion and catalytic performance, can significantly improve PEC performances.
However, TiO2Energy gap is larger, can only be therefore relatively low in visible region photoelectric transformation efficiency by ultraviolet excitation.In this reality
In testing, Cu-Co-Fe can promote the transmission of electronics, reduce the compound of electron-hole pair, improve as metal oxide catalyst
Photoelectric current, and polylysine is big as polymer, specific surface area, as excellent fixation matrix, can strengthen the absorption of antibody
Amount, improve the sensitivity of immunosensor.The present invention is situated between by a simple one-step synthesis method rutile-type sees crystal
（RTM）And a typical sensitizer polylysine is introduced further to improve RTM photoelectric transformation efficiency.Antigen is special with antibody
The opposite sex combines, and forms space steric effect, will significantly reduce photo-signal.Photo-signal and zearalenone concentration
It is linear within the specific limits, realize the highly sensitive detection of zearalenone.
The content of the invention
The purpose of the present invention is sensitized altogether based on polylysine and Nanometer Copper ferro-cobalt for a kind of of zearalenone
TiO2Jie sees the preparation method of the label-free type optical electro-chemistry sensor of crystal.
To realize goal of the invention, the present invention adopts the following technical scheme that：
(1) GCE pretreatment：GCE mechanical grindings first on the chamois leather for be covered with alumina powder are polished, and table is washed away with secondary water
Face residual powder, then move into ultrasonic water bath and clean, until cleaning up, ethanol is finally sequentially used, diluted acid and water thoroughly wash；
（2）The preparation of PL/Cu-Co-Fe/RTM/Ab/ZEN modified electrodes：It is 3mg/ml rutile TiOs that 4 μ L concentration, which are added dropwise,2
It is situated between and sees crystal（RTM）Suspension is dried under clean glassy carbon electrode surface, infrared lamp, is cooled to room temperature, and 4 μ L concentration are added dropwise
Dried for 3mg/mL RTM suspension under clean glassy carbon electrode surface, infrared lamp, be cooled to room temperature, it is then that 4 μ L are dense
It is 1 mg/ mLCu-Co-Fe solution drop coatings to the electrode surface of modified to spend, and Drying and cooling produces to room temperature under infrared lamp
To Cu-Co-Fe/RTM modified electrodes；It is again that 3mg/mL polylysin solution drop coating to the electrode surface modified, drying is cold
But, that is, PL/Cu-Co-Fe/RTM modified electrodes are obtained；By modified electrode in concentration be 1 mg/mL Ab solution under 37 °C
50 min are incubated, then remove unnecessary Ab using pH 6.5 phosphate buffer solution, then it is 1.0 that electrode is immersed into concentration
The wt.% h of BSA 1, on enclosed-electrode surface nonspecific activity site, after washing away surface residual liquid, that is, obtains PL/Cu-Co-
Fe/RTM/ Ab modified electrodes；Electrode is immersed in the ZEN standard liquids of 5 μ L various concentrations 25 min are incubated under 37 °C；With
PH 6.5 phosphate buffer solution rinses electrode surface and at ambient temperature naturally dry, obtains PL/Cu-Co-Fe/RTM/
Ab/ZEN modified electrodes；
（3）The detection of zearalenone：It is measured using three-electrode system, is modified with PL/Cu-Co-Fe/RTM/Ab/ZEN
Electrode is working electrode, and Ag/AgCl is reference electrode, and platinum electrode is to electrode, is detected using optical electro-chemistry work station,
Setting voltage is 0.1V, carries out switch lamp every 10s, is filtered before the monochromatic light excitation source use of xenon lamp transmitting by monochromator；
In pH 6.5 PBS cushioning liquid, detection 1 × 10 is carried out by optical electro-chemistry work station-6The systems of ng/mL -10 ng/mL mono-
The zearalenone standard liquid of row various concentrations, by recording caused different current signals before and after switch lamp, draw work
Make curve；Testing sample solution is detected instead of zearalenone standard liquid, and the result of detection can pass through working curve
Check in.
Above-mentioned rutile TiO2It is situated between and sees crystal（RTM）The preparation of material：
0.5 g neopelexes（SDBS）It is dissolved in the mol/mL HNO of 25 mL 2.23In solution, stir 15 minutes.
Then 0.5 mL isopropyl titanates are added（IV）, 48 h are stirred under 80 °C.Then, products therefrom through centrifuging, with ultra-pure water, ethanol
After washing 4-5 times, it is dried overnight under 60 °C.Above-mentioned product calcines 1h to remove the organic matter of residual in 400 °C of air,
Rutile TiO is made2It is situated between and sees crystal.
Above-mentioned copper ferro-cobalt material（Cu-Co-Fe）Preparation：
By glass-carbon electrode（The mm of GCE, φ=5）Polished successively with 6 μm, 1 μm, 0.05 μm of alumina powder on chamois leather, with two
Secondary water rinses, then the ultrasonic 5min in redistilled water；By treated electrode be immersed in containing 0.25mol/L potassium nitrate,
1.25 × 10-4 mol/L copper sulphate, 1.25 × 10-4 mol/L potassium ferricyanides mixed solution in, made with platinum electrode to electrode,
Ag/AgCl is reference electrode, and potential window is 0.0 V of V to+1.0, in the case where 50 mV/s sweep speed scan round 30 enclose, by electrode
Taking-up is rinsed with secondary water, then the stripping down from electrode surface by sediment, is smashed to pieces, vacuum drying, copper ferro-cobalt material is made；
A certain amount of copper ferro-cobalt solid is weighed, 100mg copper ferro-cobalt solids are scattered in the 10mL aqueous solution, that is, being configured to concentration is
10mg/mL Cu-Co-Fe solution；It is ultrasonic in Ultrasound Instrument again, suspension is obtained, 10 μ L 10mg/ is drawn with liquid-transfering gun
MLCu-Co-Fe suspension, then diluted with 90 μ L secondary waters, you can obtain 1mg/mL Cu-Co-Fe solution.
One kind of the present invention is based on TiO2It is situated between and sees the zearalenone optical electro-chemistry sensor of crystal, including work
It is reference electrode to electrode and Ag/AgCl that electrode, platinum electrode, which are, it is characterised in that described working electrode uses PL/Cu-
Co-Fe/RTM/Ab/ZEN modified electrodes, it is prepared by the method for following step, 1）The polishing of glass-carbon electrode：Glass carbon
Electrode mechanical grinding first on the chamois leather for be covered with alumina powder polishes, and washes away remained on surface powder with secondary water, then move into
Cleaned in ultrasonic water bath, until cleaning up, finally sequentially use ethanol, diluted acid and water thoroughly wash；2）PL/Cu-Co-Fe/
The preparation of RTM/Ab/ZEN modified electrodes：It is 3mg/ml rutile TiOs that 4 μ L concentration, which are added dropwise,2It is situated between and sees crystal（RTM）Suspension
Dried under clean glassy carbon electrode surface, infrared lamp, be then 1 mg/mLCu-Co-Fe solution drop coating to repairing by 4 μ L concentration
The electrode surface adornd, under infrared lamp Drying and cooling obtains Cu-Co-Fe/RTM modified electrodes to room temperature；Again by 4 μ L
3mg/mL polylysin solution drop coating Drying and cooling, that is, obtains PL/Cu-Co-Fe/RTM modifications to the electrode surface modified
Electrode；Modified electrode is incubated 50 min in the Ab solution that concentration is 1 mg/mL under 37 °C, then using pH's 6.5
Phosphate buffer solution removes unnecessary Ab, then electrode immersed into the h of BSA 1 that concentration is 1.0 wt.%, non-on enclosed-electrode surface
Activity specific site, after washing away surface residual liquid, that is, obtain PL/Cu-Co-Fe/RTM/ Ab modified electrodes；Electrode is immersed 5
25 min are incubated under 37 °C in the ZEN standard liquids of μ L various concentrations；Electrode table is rinsed with pH 6.5 phosphate buffer solution
Face and at ambient temperature naturally dry, obtain PL/Cu-Co-Fe/RTM/ Ab/Ag modified electrodes；
One kind of the present invention is based on TiO2It is situated between and sees detection side of the optical electro-chemistry sensor for zearalenone of crystal
Method, it is characterised in that step is as follows：1）It is measured using three-electrode system, is modified with PL/Cu-Co-Fe/RTM/Ab/ZEN
Electrode is working electrode, and Ag/AgCl is reference electrode, and platinum electrode is to electrode, is detected using optical electro-chemistry work station,
Setting voltage is 0.1V, carries out switch lamp every 10s, is filtered before the monochromatic light excitation source use of xenon lamp transmitting by monochromator；
2）In pH 6.5 PBS cushioning liquid, detection 1 × 10 is carried out by optical electro-chemistry work station-6Ng/mL -10 ng/mL mono-
The zearalenone standard liquid of the different solubility of series, by recording caused different current signals before and after switch lamp, draw
Working curve；Testing sample solution is detected instead of zearalenone standard liquid, and the result of detection can be bent by working
Line checks in.
The present invention remarkable advantage be：
(1) rutile TiO being sensitized with polylysine2Being situated between, to see crystal be photoelectric activity base material, rutile TiO2It is situated between
Seeing crystal has higher porosity, and the introducing of polylysine enhances the transmission speed of electronics, with single conventional Ti O2It is single
Brilliant material is compared, and effectively improves the sensitivity of photoelectric transformation efficiency and sensor.Using the compound as Electrophotosensitive interface, keep away
Exempt from the preparation of the photoelectricity probe of complexity, realize the label-free type detection for zearalenone.
(2) antigen combines to form space steric effect with antibody specificity, and obtained sensor is realized to Gibberella zeae
The super sensitivity detection of ketenes.
Brief description of the drawings
Fig. 1 is the preparation process signal of the label-free type optical electro-chemistry sensor of zearalenone of the present invention
Figure.
Fig. 2 A are various concentrations 1 × 10-6ng/mL–10 ng/mL（a-i）Zearalenone standard liquid, sensing electricity
The photocurrent response figure of pole.
Fig. 2 B are linear relationship chart of the photocurrent response with zearalenone concentration of standard solution of sensing electrode.
Embodiment
The present invention further illustrates the present invention with the following example, but protection scope of the present invention is not limited to following reality
Apply example.
Rutile TiO used in following embodiments2It is situated between and sees crystal（RTM）The preparation of material：
0.5 g neopelexes（SDBS）It is dissolved in the mol/mL HNO of 25 mL 2.23In solution, stir 15 minutes.
Then 0.5 mL isopropyl titanates are added（IV）, 48 h are stirred under 80 °C.Then, products therefrom through centrifuging, with ultra-pure water, ethanol
After washing 4-5 times, it is dried overnight under 60 °C.Above-mentioned product calcines 1h to remove the organic matter of residual in 400 °C of air,
Rutile TiO is made2It is situated between and sees crystal.
Copper ferro-cobalt material used in following embodiments（Cu-Co-Fe）Preparation：
By glass-carbon electrode（The mm of GCE, φ=5）Polished successively with 6 μm, 1 μm, 0.05 μm of alumina powder on chamois leather, with two
Secondary water rinses, then the ultrasonic 5min in redistilled water.By treated electrode be immersed in containing 0.25mol/L potassium nitrate,
1.25×10-4Mol/L copper sulphate, 1.25 × 10-4In the mixed solution of the mol/L potassium ferricyanides, made with platinum electrode to electrode,
Ag/AgCl is reference electrode, and potential window is 0.0 V of V to+1.0, in the case where 50 mV/s sweep speed scan round 30 enclose, by electrode
Taking-up is rinsed with secondary water, then the stripping down from electrode surface by sediment, is smashed to pieces, vacuum drying, copper ferro-cobalt solid is made
Material.A certain amount of copper ferro-cobalt solid material is weighed, 100mg copper ferro-cobalt solid materials are scattered in 10mL secondary waters, that is, matched somebody with somebody
It is set to the Cu-Co-Fe solution that concentration is 10mg/mL；It is ultrasonic in Ultrasound Instrument again, suspension is obtained, 10 μ L are drawn with liquid-transfering gun
Suspension, then they are diluted with 90 μ L secondary waters, you can obtain 1mg/mL Cu-Co-Fe solution.
Embodiment 1
One kind is based on TiO2Jie sees the preparation method (as shown in Figure 1) of the label-free optical electro-chemistry sensor of crystal：
（1）The pretreatment of glass-carbon electrode：Glass-carbon electrode mechanical grinding first on the chamois leather for be covered with alumina powder polishes, and uses
Secondary water washes away remained on surface powder, then moves into ultrasonic water bath and clean, until cleaning up, finally sequentially uses ethanol, diluted acid
Thoroughly washed with water；
（2）4 μ L concentration are added dropwise to dry under clean glassy carbon electrode surface, infrared lamp for 3 mg/mL RTM suspension, cool down
To room temperature；
（3）Again by the mg/mL of 4 μ L 1 Cu-Co-Fe solution drop coating to the electrode surface modified, it is placed under infrared lamp and dries
It is dry, then cool down at room temperature；
（4）Then 4 μ L 3mg/mL polylysin solution drop coating Drying and cooling, that is, is obtained to the electrode surface modified
PL/Cu-Co-Fe/RTM modified electrodes；
（5）By modified electrode in Ab11h is incubated under 37 °C in (2 mg/mL) solution, then the phosphoric acid buffer with pH 6.5 is molten
Liquid washes away unnecessary Ab and electrode is immersed into the h of BSA 1 that concentration is 1.0 wt.%, nonspecific activity on enclosed-electrode surface again
Site；After washing away surface residual liquid, electrode is immersed in the ZEN standard liquids of 5 μ L various concentrations and be incubated 1h under 37 °C；With
PH 6.5 phosphate buffer solution rinses electrode surface and at ambient temperature naturally dry, and PL/Cu-Co-Fe/RTM/ is made
Ab/ZEN modified electrodes.
Embodiment 2
One kind is based on TiO2It is situated between and sees detection method of the optical electro-chemistry sensor for zearalenone of crystal, step is as follows：
（1）It is measured using three-electrode system, with PL/Cu-Co-Fe/RTM/Ab/ZEN modified electrodes made from embodiment 1
For working electrode, Ag/AgCl is reference electrode, and platinum electrode is to electrode, is detected, set using optical electro-chemistry work station
Voltage is 0.1V, carries out switch lamp every 10s, is filtered before the monochromatic light excitation source use of xenon lamp transmitting by monochromator；
（2）In pH 6.5 PBS cushioning liquid, detection 1 × 10 is carried out by optical electro-chemistry work station-6 ng/mL–10
A series of zearalenone standard liquid of various concentrations of ng/mL, believed by caused different electric currents before and after recording switch lamp
Number, drawing curve.Fig. 2 A are various concentrations 1 × 10-6ng/mL–10 ng/mL（a-i）Zearalenone standard is molten
Liquid, the photocurrent response of sensing electrode.Fig. 2 B are the photocurrent response and zearalenone concentration of standard solution of sensing electrode
Linear relationship chart.
Testing sample solution is detected instead of zearalenone standard liquid, the result of detection can be bent by working
Line checks in.
Claims (5)
1. the preparation method of the label-free type optical electro-chemistry sensor of a kind of zearalenone, it is characterised in that including following
Step：
（1）Glass-carbon electrode（GCE）Pretreatment：GCE mechanical grindings first on the chamois leather for be covered with alumina powder polish, and use
Secondary water washes away remained on surface powder, then moves into ultrasonic water bath and clean, until cleaning up, finally sequentially uses ethanol, diluted acid
Thoroughly washed with water；
（2）The preparation of PL/Cu-Co-Fe/RTM/Ab modified electrodes：The rutile TiO that 4 μ L concentration are 3mg/ml is added dropwise2It is situated between
See crystal（RTM）Suspension is dried under clean glassy carbon electrode surface, infrared lamp, is cooled to room temperature, then by 4 μ L's
1mg/ml Cu-Co-Fe solution drop coatings are to the electrode surface of modified, and Drying and cooling is to room temperature under infrared lamp；Again in the modification
The μ L concentration of electrode surface drop coating 3 is 3mg/ml polylysin solution, that is, obtains PL/Cu-Co-Fe/RTM modified electrodes；Most
Eventually, the modified electrode obtained is soaked in 1 mg/mL zearalenone antibody-solutions, 50 min are incubated under 37 °C,
Then unnecessary zearalenone antibody A b is removed using pH 6.5 phosphate buffer solution,It is by electrode immersion concentration again
1.0 wt.% bovine serum albumin(BSA)（BSA）The h of solution 1, on enclosed-electrode surface nonspecific activity site, and it is residual to wash away surface
After extraction raffinate, that is, obtain PL/Cu-Co-Fe/RTM/Ab modified electrodes；
（3）The preparation of PL/Cu-Co-Fe/RTM/Ab/ZEN modified electrodes：PL/Cu-Co-Fe/RTM/Ab modified electrodes are immersed
The zearalenone of various concentrations（ZEN）In standard liquid 25min is incubated under 37 °C；With pH 6.5 phosphate buffer solution
Electrode surface and at ambient temperature naturally dry are rinsed, obtains PL/Cu-Co-Fe/RTM/Ab/ZEN modified electrodes；
（4）The detection of zearalenone：It is measured using three-electrode system, is repaiied with PL/Cu-Co-Fe/RTM/Ab/ZEN
Decorations electrode is working electrode, and Ag/AgCl is reference electrode, and platinum electrode is to electrode, is examined using optical electro-chemistry work station
Survey, setting voltage is 0.1V, switch lamp is carried out every 10s, by monochromator mistake before the monochromatic light excitation source use of xenon lamp transmitting
Filter；In pH 6.5 PBS cushioning liquid, detection 1 × 10 is carried out by optical electro-chemistry work station-6Ng/mL -10 ng/mL it
Between a series of various concentrations zearalenone standard liquid, believed by recording caused different electric currents before and after switch lamp
Number, drawing curve；Testing sample solution is detected instead of zearalenone standard liquid, and the result of detection can pass through
Working curve checks in.
2. according to the method for claim 1, it is characterised in that described rutile TiO2It is situated between and sees crystal（RTM）Material by
Prepared by following methods：0.5 g neopelexes（SDBS）It is dissolved in the mol/mL HNO of 25 mL 2.23In solution,
Stirring 15 minutes；Then 0.5mL isopropyl titanates are added（IV）, 48 h are stirred under 80 °C；Then, products therefrom is through centrifuging, using
After ultra-pure water, ethanol wash 4-5 times, it is dried overnight under 60 °C；It is residual to remove that above-mentioned product calcines 1h in 400 °C of air
The organic matter stayed, rutile TiO is made2It is situated between and sees crystal（RTM）.
3. described method is required according to right 1, it is characterised in that described copper ferro-cobalt material (Cu-Co-Fe) is by following methods
Prepare：By glass-carbon electrode（The mm of GCE, φ=5）Polished successively with 6 μm, 1 μm, 0.05 μm of alumina powder on chamois leather,
Rinsed with secondary water, then the ultrasonic 5min in redistilled water；Treated electrode is immersed in containing 0.25mol/L nitric acid
Potassium, 1.25 × 10-4 mol/L copper sulphate, 1.25 × 10-4 mol/L potassium ferricyanides mixed solution in, opposed electricity with platinum electrode
Pole, Ag/AgCl are reference electrode, and potential window is 0.0 V of V to+1.0, in the case where 50 mV/s sweep speed scan round 30 enclose, will
Electrode taking-up is rinsed with secondary water, then the stripping down from electrode surface by sediment, is smashed to pieces, vacuum drying, copper ferro-cobalt is made
Material；A certain amount of copper ferro-cobalt solid is weighed, 100mg copper ferro-cobalt solids are scattered in the 10mL aqueous solution, that is, are configured to concentration
For 10mg/mL Cu-Co-Fe solution；It is ultrasonic in Ultrasound Instrument again, suspension is obtained, 10 μ L 10mg/ is drawn with liquid-transfering gun
MLCu-Co-Fe suspension, then diluted with 90 μ L secondary waters, you can obtain 1mg/mL Cu-Co-Fe solution.
4. a kind of label-free type optical electro-chemistry sensor of zearalenone, including working electrode, platinum electrode are to electrode
It is reference electrode with Ag/ AgCl, it is characterised in that described working electrode is modified using PL/Cu-Co-Fe/RTM/Ab/Ag
Electrode, its be prepared by the method for following step 1）The polishing of glass-carbon electrode：Glass-carbon electrode is being covered with alumina powder first
Mechanical grinding polishing, remained on surface powder is washed away with secondary water on the chamois leather at end, then is moved into ultrasonic water bath and cleaned, until cleaning
Totally, ethanol is finally sequentially used, diluted acid and water thoroughly wash；2）The preparation of PL/Cu-Co-Fe/RTM/Ab/Ag modified electrodes：
4 μ L concentration are added dropwise to dry under clean glassy carbon electrode surface, infrared lamp for 3mg/mL RTM suspension, are cooled to room temperature,
Then it is electrode surface of the 1 mg/mLCu-Co-Fe solution drop coating to modified by 4 μ L concentration, Drying and cooling is extremely under infrared lamp
Room temperature, that is, obtain Cu-Co-Fe/RTM modified electrodes；Again by 3mg/mL polylysin solution drop coating to the electrode table modified
Face, Drying and cooling, that is, obtain PL/Cu-Co-Fe/RTM modified electrodes；By modified electrode in 1 mg/mL Ab solution in 37 °
50 min are incubated under C, then remove unnecessary Ab using pH 6.5 phosphate buffer solution,It is 1.0 that electrode is immersed into concentration again
The wt.% h of BSA 1, on enclosed-electrode surface nonspecific activity site, after washing away surface residual liquid, that is, obtains PL/Cu-Co-
Fe/RTM/ Ab modified electrodes；Electrode is immersed in the ZEN standard liquids of various concentrations 25 min are incubated under 37 °C；Use pH
6.5 phosphate buffer solution rinses electrode surface and at ambient temperature naturally dry, obtains PL/Cu-Co-Fe/RTM/ Ab/
ZEN modified electrodes.
5. one kind described in claim 4 is based on TiO2It is situated between and sees inspection of the optical electro-chemistry sensor for zearalenone of crystal
Survey method, it is characterised in that step is as follows：1）It is measured using three-electrode system, with PL/Cu-Co-Fe/RTM/Ab/ZEN
Modified electrode is working electrode, and Ag/AgCl is reference electrode, and platinum electrode is to electrode, is carried out using optical electro-chemistry work station
Detection, setting voltage is 0.1V, switch lamp is carried out every 10s, by monochromator before the monochromatic light excitation source use of xenon lamp transmitting
Filtering；2）In pH 6.5 PBS cushioning liquid, detection 1 × 10 is carried out by optical electro-chemistry work station-6 ng/mL–10 ng/
A series of zearalenone standard liquid of different solubility between mL, by recording caused different electric currents before and after switch lamp
Signal, drawing curve；Testing sample solution is detected instead of zearalenone standard liquid, and the result of detection can lead to
Working curve is crossed to check in.
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| CN111077201A (en) * | 2019-12-23 | 2020-04-28 | 江苏大学 | Preparation method of photoelectrochemical aptamer sensor for monitoring zearalenone |
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