We investigated the radiocarbon age and stable isotope composition of bioapatite from bone, enamel, and dentine material from 3 different species of extinct mammals in South America. Most samples of Eremotherium laurillardi, Toxodon platensis, and Notiomastodon platensis were collected in natural depressions located in the northeastern Brazilian provinces of Sergipe, Bahia, and Rio Grande do Norte. All samples studied were devoid of collagen, which had decomposed as a result of high microbiological activity in this tropical region. We have instead analyzed the bioapatite fraction of the samples, which was relatively well preserved even in these harsh tropical conditions. The mineral fraction of bone and tooth material does not usually undergo microbiological decomposition but may be exposed to isotopic exchange with environmental carbonates. The problem thus becomes one of separating the diagenetic carbonates without destroying the bioapatite. We offer a technique for removing the secondary diagenetic carbonates by treatment with diluted acetic acid in a vacuum. We also demonstrate that proper pretreatment of bone and tooth samples allows the separation of diagenetic carbonates from bioapatite, as long as the carbon in these samples has not degraded completely. Bone, enamel, and dentine samples from individuals of the 3 mammalian species were dated using this technique and were compared to results by other researchers from the literature. Date ranges for the species presented were in good agreement with prior research. A comparison with other dating techniques such as U/Th and ESR shows the reliability of the treatment described and the feasibility of 14C dating the bioapatite fraction given certain conditions. In 2 cases, we dated bone enamel and dentine samples from the same individuals of N. platensis, with results between 14 and 21 ka. Results from dating samples of T. platensis are between 11.5 and 13 ka. The oldest tissue in both cases was dentine. The dating of enamel and dentine from the same species did not show regular differences; however, more often the dentine material was older. The oldest date, ≃22.5 ka for E. laurillardi, was obtained on the bioapatite fraction of dentine.