Fe3O4@PPy,a kind of magnetic nanoparticles modified by polypyrrole,is synthesized.A method for detecting polychondroitin sulfate in heparin is developed through combining Fe3O4@PPy with tetraphenylvinyl derivatives(TTAPE),an AIE fluorescent probe.The movement of heparin and chondroitin polysulfate is restricted when they bind to TTAPE,thus release fluorescence,while Fe3O4@PPy can quench the fluorescence.The fluorescence enhancement law when heparin and chondroitin polysulfate combine with TTAPE is studied,and the fluorescence quenching law by Fe3O4@PPy is also studied.Different quenching curves are established to detect heparin and chondroitin polysulfate simultaneously.It is confirmed through experiments that the best fluorescence detection wavelength for heparin and chondroitin polysulfate is 482 nm both,the dosage of Fe3O4@PPy is 5 mg,the linear range of detection concentration is 0-3.5 mg·L-1,the relative deviation of heparin concentration is less than 0.5%.The recoveries of polychondroitin sulfate in actual heparin samples are 90%and 96.67%,the relative standard deviations are 4.4%and 4.1%,respectively.