A LC/MS Method for the Determination of Cyanobacteria Toxins in Water

The cyanobacteria toxins anatoxin-a, microcystin-LR, microcystin-RR, microcystin-YR, and nodularin were separated in less than 30 min on several 1 mm × 15 cm reversed-phase liquid chromatography (LC) columns, and their electrospray mass spectra were measured using injections of 50 ng or less with a benchtop time-of-flight (TOF) mass spectrometer. New data from this work include the following: (a) the impact of acetic acid concentrations in the methanol−water mobile phase on measured ion abundances; (b) the performance of the electrospray-TOF mass spectrometer as an LC detector; (c) the accuracy and precision of exact m/z measurements after LC separation with a routinely used mass spectrometer resolving power of 5000; and (d) recoveries of the five toxins from reagent water, river waters, and sewage treatment plant effluent samples extracted with C-18 silica particles enmeshed in thin Teflon membrane filter disks. This technique has the potential of providing a relatively simple and reasonable-cost sample preparation and LC/MS method that provides the sensitivity, selectivity, reliability, and information content needed for source and drinking water occurrence and human exposure studies.