The variation of dissolved and particulate metal(loid) concentrations was investigated during a Mediterranean flood in a former mining watershed, the Gardon River (SE France), using high-temporal resolution sampling. Dissolved antimony originating from the Upper Gardon River watershed underwent dilution during flood. Conversely, dissolved As and particulate As, Pb, Zn, Cd and Tl concentrations exhibited increased values during rising flood compared to low and receding flow conditions, with a double-peak shape. As, Pb, Cd and Tl concentration data in suspended particulate matter from this double-peak were distributed along two different correlation lines, showing the successive mobilization of two groups of particles highly enriched with As and Cd or Pb and Tl, both inherited from ancient Pb/Zn mines. Metal(loid) loads during the monitored 24 h-flood event were: 0.5 kg for Cd, 19.4 kg for Sb and 204 kg for As in the dissolved phase and 24 kg for Cd, 38 kg for Tl, 94 kg for Sb, 1915 kg for As, 2860 kg for Pb and 5214 kg for Zn in the particulate phase. Altogether, these results highlighted the importance of floods in the mobilization of metals and metalloids from ancient mining sites in Mediterranean regions, showing the need for high-temporal resolution monitoring of flood events to accurately assess the long-term contribution of mining activity to metal(loid) loads of downstream watershed.Please cite this article as: Resongles, E., et al., Variation of dissolved and particulate metal(loid) (As, Cd, Pb, Sb, Tl, Zn) concentrations under varying discharge during a Medite.