This work proposes a novel method to determine the Cd(II) and Cr(III) content in commercial sugar samples. It is based on the extraction of the analytes (as ammonium pyrrolidine dithiocarbamate complexes) into a semipermeable membrane device (SPMD) filled with CHCl3. After extraction, the SPMD was deployed and opened, and the analytes were recovered from the organic phase by back extraction with a 4.2 mol L−1 HNO3 solution. The analytes present in the acid extract were measured with graphite furnace atomic absorption spectrometry. Under optimized conditions, the limit of quantification of the method was 1.2 and 3.1 ng g−1 for Cd(II) and Cr(III), respectively. Twelve samples of different types of sugar were analyzed. In addition, a recovery test was performed to evaluate the accuracy of the method. The recovery percentage was 90 %–102 % for Cd(II) and 85.2 %–103 % for Cr(III).
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