An analytical procedure based on matrix solid-phase dispersion (MSPD) and liquid chromatography-mass spectrometry (LC-MS) was developed for determining three microcystins (MCs) in natural water blooms and cyanobacteria strain cultures. The procedure involves sample homogenization with C(18), washed with dichloromethane to eliminate interfering compounds, and elution with acidic methanol. Results were compared to those achieved by using an organic solvent standard method. Mean recoveries of MCs with MSPD were 85-92% with intra-day relative standard deviation (RSDs) of 9-19%, whereas organic solvent extraction resulted in recovery rates of 92-105% with intra-day RSDs ranging from 8 to 18%. Limits of quantification (LOQs) were 1 microg g(-1) dry weight for the MCs either by MSPD or organic solvent extraction. The two analytical methods tested were specific and sensitive to the extraction of MCs and were applied to the detection of MCs in water blooms and culture strains. The concentration of MCs varied from 7 to 3,330 microg g(-1) of lyophilized cells with MC-LR always showing the highest concentration. MCs levels were higher in culture strains than in water blooms, except for MC-LR, whose concentration in blooms was slightly superior to that determined in culture strains.