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There is interest in measuring total mercury (THg) and methylmercury (MeHg) in dried blood spots (DBS) though more research is required to evaluate mercury (Hg) speciation in DBS and to validate the agreement between blood sources (venous vs capillary) and matrices (whole blood vs DBS). Therefore, the present study aimed to develop, evaluate, and validate a DBS-based method to assess MeHg and inorganic mercury (InHg) exposure in human population studies. First, we used volume-controlled (40 μL) paired DBS-whole blood samples to develop