DOI: 10.3724/SP.J.1096.2013.30393

Chinese Journal of Analytical Chemistry (分析化学) 2013/41:12 PP.1844-1850

Determination of Five Microcystins in Cyanobacteria by Liquid Chromatography Tandem Mass Spectrometry Using Freezing-thawing and Solid Phase Extraction

A method was developed for simultaneous determination of five microcystins(MCs) in Cyanobacteria by liquid chromatography Tandem mass spectrometry(LC-MS/MS) using freezing-thawing and solid phase extraction(SPE). Cyanobacteria in environmental water was collected by 0.45 μm hybrid filter and extracted with two times of 5 mL 75% methanol after three times of -20℃/37℃ freezing-thawing. The extract was concentrated by end-capped C18 SPE cartridge with a clean-up by 10 mL 5% methanol. Five MCs were detected by LC-MS/MS with multiple reaction monitoring and external standard method. Gradient elution was employed with a mobile phase consisting of acetonitrile with 0.1% formic acid and water with 0.1% formic acid on C18 column (50 mm×2.1 mm, 1.7 μm). The method showed good linear correlations in a range of 1.25-50 μg/L with correlation coefficients greater than 0.995. RSD and LOD were 3.0%-11.5% and 0.05-0.2 ng, respectively. Recovery of three spiked levels (1, 5 and 50 ng) for five MCs were 63.7%-100.4% (RSD 5.5%-13.1%), 72.6%-85.7% (RSD 3.1%-6.6%) and 72.5%-80.5% (RSD 2.6%-8.3%), respectively. The proposed method was applied in the detection of intracellular and extracellular MCs in one drinking water source of South China from August to December.

Key words:Microcystin,Liquid chromatography Tandem mass spectrometry,Cyanobacteria,Freezing-thawing,Solid phase extraction

ReleaseDate:2015-04-19 11:08:01

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