Abstract. The literature on the speciation of metal ions in biological fluids is comprehensively reviewed. Critical examination on this subject reveals that major work has been done in blood and urine. Speciation in materials like milk has not yet been widely studied. On the other hand, only few references could be found on sweat, saliva, cell lysate, cerebrospinal, seminal, tear and bronchoalveolar fluids. The topics studied for these fluids were mainly the speciation of arsenic, mercury, aluminium and selenium. Work on the speciation of other elements like zinc, chromium, cadmium, lead, copper, iron etc. have also been carried out in such matrices. The present literature survey includes also a critical comment about the sampling and storage of the fluids, general methodologies and analytical details of the developed methods for studying such metal ion speciation.