Simultaneous Determination of Seven Microcystins in Aquatic Product by High Performance Liquid Chromatography-Tandem Mass Spectrometry
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Abstract:
A new analytical method for the simultaneous determination of seven microcystins (MC-RR, MC-YR, MC-LR, MC-LA, MC-LW, MC-LF and MC-LY) in aquatic product by high performance liquid chromatography-tandem mass spectrometry (LC-MS-MS) was established. Aquatic product sample was extracted with 90% methanol (V/V), and then the extracts were cleaned up by SPE and analyzed by LC-MS-MS using a C18 column, employing 0.1% formic acid acetonitrile solution - 0.1% formic acid aqueous solution as the mobile phase for gradient elution. Mass spectrum was used for assistant identification. External standard method was applied for quantization. The result indicated that the limits of quantification (LOQs) of seven microcystins were ranged from 0.2 μg/kg to 0.5 μg/kg. Meanwhile, the linear correlation coefficients (r> 0.999 0) of seven microcystins were obtained within the irrespective linear ranges. The recoveries of seven microcystins from spiked samples at the spiking levels of 1.0-20 μg/kg were ranged from 71.5 to 106 % with RSD of 3.2 %- 9.1% (n=6). The method was simple, precise and had high recoveries for the determination of microcystins in aquatic product samples.
