A dual-cloud point extraction (d-CPE) procedure was developed for the simultaneous preconcentration and determination of trace level Se in food samples by hydride generation-atomic fluorescence spectrometry (HG-AFS). The Se(IV) was complexed with ammonium pyrrolidinedithiocarbamate (APDC) in a Triton X-114 surfactant-rich phase, which was then treated with a mixture of 16% (v/v) HCl and 20% (v/v) HO. This converted the Se(IV)-APDC into free Se(IV), which was back extracted into an aqueous phase at the second cloud point extraction stage. This aqueous phase was analyzed directly by HG-AFS. Optimization of the experimental conditions gave a limit of detection of 0.023μgL with an enhancement factor of 11.8 when 50mL of sample solution was preconcentrated to 3mL. The relative standard deviation was 4.04% (c=6.0μgL, n=10). The proposed method was applied to determine the Se contents in twelve food samples with satisfactory recoveries of 95.6-105.2%.

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