The invention relates to a method and a device for detecting a polymer film ion selective electrode. The method comprises the following steps of : putting a nucleic acid aptamer and polycation into a detection pond, and inserting a polycation selective electrode into the detection pond to generate a comparison signal; adding the nucleic acid aptamer into the detection tank, reacting with standard solution of a substance to be detected, adding the polycation, and inserting the polycation selective electrode into the detection pond to generate standard signals of the standard solution of the substance to be detected at different concentrations; obtaining a standard curve according to the standard signals and the comparison signal; adding liquid to be detected into the detection pond, adding the nucleic acid aptamer, reacting with the liquid to be detected, adding the polycation in the ratio to conduct the signals, and inserting the polycation selective electrode into the detection pond to generate a sample signal; and acquiring a signal to be detected according to the sample signal and the comparison signal, and acquiring the concentration of the liquid to be detected by the reference of the standard curve. The method is wide in application range, high in generality, large in electrode response signals and obvious in potential change, so the method is a marking-free and immobilization-free method.
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