Objective To develop a method for simple and rapid determination of 2-methyl-3-methoxy-4-phenylbutyric acid (MMPB), an oxidation and hydrolyzation product of microcystin (MC) in water using gas chromatography-mass spectrometry (GC-MS).
Methods Samples were oxidized with potassium permanganate, extracted using n-hexane, then derivatized with hexafluoroisopropanol (HFIP)/N, N'-diisopropylcarbodiimide (DIC), and finally detected by GC-MS and quantified using internal standard method.
Results The method was validated in terms of method detection limit (MDL) (0.101 μg/L), linearity range (0.2-10.0 μg/L), accuracy (80%-120%), precision (relative standard deviation, RSD<15%), and repeatability (RSD<15%). The representative samples were successfully detected with concentrations between < MDL and 3.090 μg/L.
Conclusion The proposed method as an alternative method of HPLC-MS/MS is practicable for the routine analysis of total microcystins in water.
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