Double-amplification electrochemiluminescence sensor and method for determining chlorpyrifos
A chlorpyrifos and sensor technology, applied in the field of pesticide residue determination, can solve problems such as a single signal amplification method, and achieve the effect of improving detection selectivity, low density, and high sensitivity detection
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Embodiment 1
[0027] The preparation of embodiment 1 hollow Fe / Co-MOF:
[0028] (1) Synthesis of PS spheres: 30 mL ultrapure water was placed in a three-necked flask, N 2 After deoxygenation, 1.5 g of polyvinylpyrrolidone (PVP) and 0.015 g of potassium persulfate were added in sequence, and after complete dissolution, 3 mL of styrene was added and heated at 70 °C for 24 h. Wash with water and ethanol and separate the product, disperse the product in 5 mL of ethanol to obtain a PS sphere dispersion, add 0.5 g of PVP to the dispersion and stir for 12 h, after the reaction is complete, the product is fully washed with ethanol and methanol, and then dispersed in 10 mL of methanol solution to obtain methanol solution of PVP-modified PS spheres;
[0029] (2) Synthesis of FeOOH nanorods: 0.2 mL polyethyleneimine was added to 100 mL 20 mM FeCl 3 •6H 2 O solution, heated and stirred at 80 °C for 2 h, and centrifuged and washed three times with ultrapure water to obtain FeOOH nanorods. Disperse F...
Embodiment 2
[0031] Example 2 Preparation of double-amplified aptasensors:
[0032] (1) Take 3 mL of 5 mM AgNO 3 and 0.5 mL of 0.01 M luminol solution were added to a flask filled with 9.0 mL of absolute ethanol and 5.0 mL of ultrapure water, and then 0.1 mL of 0.1 M NaOH was quickly added and stirred for 4 h. When the solution color turned dark yellow, the mixture was fully washed with ethanol, and the product was dispersed in 5 mL of ethanol to obtain a Lu-Ag ethanol solution;
[0033] (2) Add 1 mL of 0.125 g / L Fe / Co-MOF ethanol solution and 500 μL Lu-Ag ethanol solution into the flask. Shake on a shaker for 30 min, then incubate at 4 °C for 12 h. A hollow Fe / Co-MOF-Lu-Ag composite was obtained. Take 80 μL of 1 μM chlorpyrifos aptamer and add to 800 μL of 0.125 g / L Fe / Co-MOF-Lu-Ag ethanol solution. Shake on a shaker for 30 min, then incubate at 4 °C for 12 h to prepare Apt-Ag-Lu-Fe / Co-MOF;
[0034] (3) The treated glassy carbon electrode GCE was plated with gold at a constant potent...
Embodiment 3
[0037] Example 3 Method for detecting chlorpyrifos with double-amplified aptasensors:
[0038] (1) Add different concentrations of chlorpyrifos pesticide dropwise on the surface of the constructed sensor, incubate at 37 °C for 1 h, and wash with PBS buffer at pH 7.8;
[0039] (2) The aptamer sensor was used as the working electrode, the Ag / AgCl electrode was used as the reference electrode, and the platinum electrode was used as the auxiliary electrode; 2 o 2 In the buffer solution of 0.1 M pH 7.8 PBS, cycle in the potential range of 0.0-0.7 V, scan the photomultiplier tube at 600 V, and record the luminous intensity;
[0040] (3) Detect the light intensity of a series of standard solutions of chlorpyrifos with different concentrations, and draw a working curve; at the same time, measure the linear range and detection limit of the sensor. The intensity of electrochemiluminescence decreases with the increase of chlorpyrifos concentration, the linear equation is DI=-359.57 lg...
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