Residue analysis of 10 aminoglycoside antibiotics in aquatic products by multiwalled carbon nanotubes combined with mixed‐mode ion exchange liquid chromatography‐tandem mass spectrometry

An ultra-high-performance liquid chromatography-tandem mass spectrometry method was developed for simultaneous determination of 10 kinds of aminoglycosides in edible parts of aquatic products. The samples were extracted with 10 mmol/L potassium dihydrogen phosphate buffer solution, then the pH value of the extract was adjusted to neutral by sodium hydroxide. Half volume of the extract was loaded onto multiwalled carbon nanotubes cartridge. All the target compounds were separated on a mixed-mode ion exchange column and detected by ultra-high-performance liquid chromatography-tandem mass spectrometry with electrospray in the positive ionization mode. Under optimized conditions, this method had a good linearity with a squared correlation coefficient > 0.999. For neomycin, the limit of detection and limit of quantification were 5.0 μg/kg and 10.0 μg/kg, respectively; for hygromycin B and apramycin, values were 2.0 μg/kg and 5.0 μg/kg, respectively; for the other seven kinds of aminoglycosides, values were 1.0 μg/kg and 2.0 μg/kg, respectively. The average recoveries presented 75.8%-107.2% with intra- and interday reproducibility ranging between 3.8% and 12.5%. The method was rapid with good separation and sharp peak shapes, had the characteristicsis of high accuracy and good precision, and was suitable for simultaneous determination of 10 kinds of aminoglycosides in aquatic products.