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The analysis of mercury in food presents a challenge for analytical chemists. Sample pre-treatment and the preconcentration of mercury prior to measurement are required, even when highly sensitive analytical methods are used. In this work, the Diffusive Gradients in Thin Films technique (DGT), combined with thermal decomposition gold amalgamation atomic absorption spectrometry (TDA-AAS), was investigated for the determination of the total dissolved mercury in fish sauces. Moreover, a new type of binding gel with Purolite S924 resin was used in DGT. Linearity assays for DGT provided determination coefficients around 0.995. Repeatability tests showed a relative standard deviation of less than 10%. pH values in the range of 3–6, as well as NaCl concentrations up to 50 g·L−1, did not affect the performance of DGT. The effective diffusion coefficient of mercury in five-fold diluted fish sauce was determined to be (3.42 ± 0.23)·10−6 cm2·s−1. Based on the 24 h deployment time of DGT, the limit of detection (LOD) for the investigated method was 0.071 µg·L−1. The proposed method, which combines DGT and TDA-AAS, allows for the analysis of fish sauces with mercury concentrations below the LOD of TDA-AAS, and significantly reduces the wear and corrosion of the TDA-AAS components.

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