Abstract: XAD-2 resin and D101 resin were compared on adsorption separation of Microcystin-LR (MC-LR) in algae crude powder. Removal effects of impurities adsorbed on these resins with microcystins (MCs) by acetic acid, acetone and ethanol were discussed at different volume fractions. It is shown that XAD-2 resin has a better purification effect than D101 resin. When MC-LR purified by XAD-2 resin is leached by acetic acid, acetone and ethanol to remove the impurities, the optimum volume fraction is 40% for acetic acid, 10% for acetone and 20% for ethanol, respectively. When eluted with 60% methanol solution, MC-LR can reach its maximum mass fraction, and this purification method is well reproducible.