Alkylphenols (APs) and bisphenols (BPs) are hazardous organic contaminants both for the environment and for mammals, including humans, where they act as endocrine disruptor compounds (EDCs) with estrogenic and cancerogenic activity. APs are toxic at very low concentrations and BPA is specifically considered a non-steroidal xenoestrogen. EDCs are present in the environment, and so the population is chronically exposed, being the diet the main exposure source. Procedures for the determination of APs and BPs in human and biological samples are scarce; therefore, a procedure for the determination of six APs and three BPs in seven human organs and tissues (kidney, liver, heart, lung, spleen, brain and abdominal fat) obtained from eight autopsies is proposed. Previously ground samples were treated by salt-assisted liquid-liquid extraction (SALLE) for isolation of the analytes. Stir bar sorptive extraction was used to preconcentrate the analytes.