Abstract:

A method for the simultaneous analysis of 14 quinolone (QN) residues in aquatic products by dispersive solidphase
extraction and liquid chromatography-tandem mass spectrometry (UPLC-MS-MS) was established. The sample was
extracted with acetonitrile (containing 5% formic acid) and followed by salting-out. Clean up of the extracts was performed
using PSA and C18 during the dispersive solid-phase extraction procedure. After evaporated to dryness under a stream of
nitrogen, the analytes were then separated on a Waters ACQUITY UPLCTM BEH C18 column (50 mm × 2.1 mm, 1.7 μm)
using binary mobile phase gradient with water containing 0.2% formic acid and methanol. The targeted compounds were
detected under a multiple reaction monitoring (MRM) mode and quantified by an external standard method. The linearity of
all 14 QNs in the range from 0.50 to 20.0 μg/L exhibited correlation coefficients greater than 0.995. The limits of detection
(LOD) and the limits of quantification (LOQ) were 0.4–1.0 and 1.0–3.0 μg/kg, respectively. The average recoveries of 14
QNs at three level spiked concentrations ranged from 82% to 90%, with relative standard deviations (n = 5) less than 11.0%.
This method was simple, rapid, sensitive and reliable, and could be applied to determine 14 QNs in aquatic products.

Key words: dispersive solid-phase extraction, ultra performance liquid chromatography-tandem mass spectrometry (UPLCMS- MS), aquatic products, quinolones