In this paper, a new technique, aqueous two-phase floatation (ATPF) which combines solvent sublation with aqueous two-phase system was used to separate and concentrate lincomycin. In the ATPF system of polyethylene glycol (PEG)/inorganic salt, the effects of solution pH, PEG molecular weight, concentration of inorganic salt in aqueous solution, nitrogen flow rate and floatation time were investigated in details, and the optimal conditions for ATPF were obtained. Under optimal conditions, the distribution ratio of ATPF was more than 118. Compared with aqueous two-phase extraction (ATPE), ATPF can not only separate and concentrate lincomycin from aqueous phase, but also efficiently reduce the wastage of PEG. The kinetics of the process of lincomycin in ATPF was also studied, and results showed it could be divided into two stages distinctly, and each stage obeyed the first-order kinetic equation. (C) 2010 Elsevier B.V. All rights reserved.