A method is described for the simultaneous determination of As (III), As (V), Sb (III) and Sb (V) in traditional Chinese medicines by hydride generation-double channel atomic fluorescence spectrometry (HG-AFS). The experimental conditions that influence the fluorescence intensities of arsenic and antimony were investigated and optimized, and the influence of foreign ions and their elimination were studied. The detection limits were found to be 0.090 3 and 0.057 8 microg x L(-1) for arsenic and antimony, respectively. The proposed method was applied to the determination of arsenic and antimony species in traditional Chinese medicines. Recoveries were in the ranges of 90.1%-105.0%, 91.3%-102.0%, 94.7%-109.0% and 98.2%-110.0% for As(III, As(V), Sb(III) and Sb(V), respectively.

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