Abstract: Through the interaction of any of the AGs i.e.the kanamycin tobramycin,or gentamycin,with titan yellow in a weakly acidic solution,low intensity of resonance rayleigh scattering spectra (RRS) given by the reactants individually was found remarkably enhanced due to the formation of an ion-association complex,which gives a new RRS spectrum.The ion association complexes formed by different aminoglycosidic antibiotics showed similar spectral characteristics,and all their RRS spectra peaks are located at 278 nm and 469 nm.Simultaneously,the frequency doubling scattering (FDS) intensity were also raised distinctly.The peaks of FDS spectra are all located at 392 nm.But no obvious change of the 2nd order scattering (SOS) was observed.Linear relationship was found between the intensity of RRS (ΔIRRS) and the concentration of aminoglycosidic antibiotics in the range from 0-5.0 μg per 10 mL of solution,but with different detection limits (3σ) from 17.2-23.3 μg·L-1.Results of test of interfering substances showed that relatively good selectivity was achieved.Based on the above findings,a RRS spectrometric method for the determination of AGs was proposed,and in its application to the analysis of AGs injection and of human blood for AGs,RSD′s (n=5) obtained were less than 3.5%,and recoveries were in the range of 96.3%-97.2%.