Extraction and high-performance liquid chromatographic method for the determination of microcystins in raw and treated waters

Abstract

Increasing concern over the presence of microcystins (cyanobacterial/blue–green algal hepatotoxins) in water supplies has emphasized the need for a suitable analytical method. As many microcystins are known to exist, a method was developed that permits the determination of numerous variants by a single procedure. The method involves filtration to separate cyanobacterial cells from water, allowing intracellular and extracellular toxin levels to be assessed. The cellular components of the samples are extracted repeatedly in methanol, which was found to be the most versatile solvent tested for the extraction of microcystins. The efficiency of this extraction procedure was found to be independent of cell biomass. The filtered water was subjected to trace enrichment using a C₁₈ solid-phase extraction cartridge, followed by identification and determination by photodiode-array high-performance liquid chromatography. The procedure was assessed using four water samples (two raw and two treated) spiked with a mixture of five microcystins and the cyanobacterial hepatotoxin nedularin. Recoveries of all but one microcystin were found to be good when spiked with concentrations as low as 250 ng l^–1. The linearity and precision of the experimental procedure were assessed for five microcystins and nodularin. The proposed method permits rapid sample processing and determination of several microcystins.