Protocol for Preconcentration and Quantification of Microcystins Using LC-MS
AssigneeThe University of Toledo
InventorsDragan Isailovic, Dilrukshika Palagama, David Baliu-Rodriguez, Bruce S. Levison, David J. Kennedy, Steven T. Haller, Kenneth Hensley
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Abstract
Methods for detecting and quantifying one or more microcystin compounds in a sample are described. The methods may include a preconcentration step, and generally utilize an LC-MS or LC-MS/MS analysis with an Orbitrap Fusion mass spectrometer or a QqQ mass spectrometer. The methods provide excellent recoveries and limits of quantification of microcystins.
Claims20
A method for detecting and quantifying a microcystin compound in a sample, the method comprising:
- purifying a sample containing a microcystin compound in plasma, serum, or urine through a solid-phase extraction to obtain a purified sample;
- conducting a quantitative analysis on the purified sample to quantify the amount of microcystin in the preconcentrated sample, wherein the quantitative analysis comprises a liquid chromatography step and a mass spectrometry step;
- and
- using a calibration curve to determine the concentration of the microcystin compound in the sample.
A method of preconcentrating mycrocystin in a sample, the method comprising:
- conditioning a solid-phase extraction (SPE) cartridge with methanol containing formic acid;
- loading a sample containing a microcystin at a first concentration onto the solid-phase extraction cartridge;
- eluting the sample with methanol containing formic acid, and collecting the eluted sample;
- evaporating solvent from the eluted sample to obtain an evaporated sample, and redissolving sample in the solvent to obtain a preconcentrated sample, wherein the preconcentrated sample contains microcystin at a second concentration, the second concentration being greater than the first concentration.
Dependencies are inferred from the claim text.