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A new method was developed for the determination of cefradine by extraction-flotation of CuSCN. The experiment indicatedthat in the presence of 0.20 mol/L NaOH the degradation of cefradine took place in water bath at 100℃. The thiol group (-SH) ofthe degradation product could reduce Cu(Ⅱ) to Cu(Ⅰ) for the formation of the emulsion CuSCN in the presence of NH