Preparation method of photoelectrochemical immunosensor for detecting prostate specific antigen
A prostate-specific, immunosensor technology, applied in the preparation of prostate-specific antigen detection and photoelectrochemical immunosensor fields, can solve the problems of low system sensitivity, reduced photoelectric conversion efficiency, etc., achieve high selectivity, increase photocurrent intensity, improve The effect of detection sensitivity
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Embodiment 1
[0019] Photosensitizer [Ir(C6) 2 (dcbpy)] + PF 6 - Synthesis and characterization of:
[0020] Weigh IrCl 3 ·3H 2 O solid (0.34g, 1mmol) was dissolved in water (5mL), stirred to fully dissolve, and coumarin-6 (0.77g, 2.2mmol) and 2-ethoxyethanol (15mL) were added to a 50mL round bottom flask refluxed at 120°C for 24 hours under the protection of nitrogen, the reaction product was naturally cooled to room temperature, the filter cake solid was collected by filtration, and then washed with water and ethanol in sequence to obtain an iridium dichloride bridged dimer product. 2,2'-bipyridine-4,4'-dicarboxylic acid (0.047 g, 0.25 mmol) and 2-ethoxyethanol (25 mL) and the resulting dimer (0.175 g, 0.1 mmol) were added to 50 mL in a round bottom flask. After stirring to dissolve, the excess Na 2 CO 3 (5mmol) was added to the above solution, stirred and heated, and refluxed under nitrogen protection for 20 hours. After the reaction was completed, the solvent was removed by di...
Embodiment 2
[0022] Preparation of the sensing working electrode:
[0023] (1) Preparation of NiO-modified ITO electrode: Put an ITO electrode (0.5cm×4.0cm) with a fixed area into 10mL ultrapure water, 10mL absolute ethanol, 10mL acetone, 10mL absolute ethanol, 10mL ultrapure water , ultrasonically cleaned for 10 minutes to remove impurities on the surface of the ITO electrode, and dried naturally. NiO nanofilms were modified on ITO electrodes by hydrothermal method. Dip the cleaned ITO glass into the configuration containing 400 μL of 0.25M Ni(NO 3 ) 2 ·6H 2O and 0.25M hexamethylenetetramine aqueous solution in a centrifuge tube, heated at 90°C for 200 minutes, cooled to room temperature, washed with ultrapure water three times, and dried under nitrogen atmosphere. Then place the ITO electrode in a muffle furnace at 350°C and keep it for 30 minutes, the heating rate is 5°C / min, and the temperature is naturally lowered to obtain a NiO-modified ITO electrode (ITO / NiO). Then it is immers...
Embodiment 3
[0025] Determination of samples:
[0026] The prepared sensing working electrode was immersed in different concentrations of PSA solutions, incubated at 37°C for 1 hour, washed and then detected by photocurrent, and the photocurrent intensity was recorded by a photoelectrochemical analyzer. The photocurrent detection adopts a three-electrode system: the prepared sensing working electrode, the platinum wire electrode as the auxiliary electrode, the Ag / AgCl electrode as the reference electrode, and the 0.1M PBS buffer solution (pH=7.4) as the detection solution under the excitation light of 475nm , the bias voltage is 0V, and the light source is turned on and off for 20s. When the PSA concentration is in the range of 1pg / mL to 10ng / mL, the photocurrent signal and the logarithm of its concentration have a good linear relationship, and the linear regression equation is ΔI=-720.151+53.800lg C PSA (pg / mL), linear correlation coefficient R 2 It was 0.9966, and the detection limit w...
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