Simultaneous Determination of Twenty-two Quinolone Residues in Eggs Using Ultra-performance Liquid Chromatography-tandem Mass Spectrometry
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Abstract:
A multiresidue method for the determination of twenty-two quinolone residues (garenoxacin, trovafloxacin, moxifloxacin, orbifloxacin, gemifloxacin, gatifloxacin, pefloxacin, ciprofloxacin, etc.) in eggs was developed based on ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). In this method, the analytes were extracted using acidified (2%) acetonitrile, degreased by n-hexane, and purified through an Oasis HLB SPE column. The twenty-two quinolones were separated on an Acquity UPLC BEH Shield RP18 column (100 mm×2.1 mm, 1.7 μm), using methanol and 0.1% formic acid as the mobile phases for gradient elution. The signals were acquired through the dual-channel multiple reaction monitoring (MRM) mode. All analytes could be well separated by using a gradient program of 11 minutes. The calibration curves of the twenty-two quinolones showed good linearity in the concentration range of 2.0~100.0 μg/L (r>0.99), and the limits of quantitation were all less than 1.0 μg/kg. The recoveries of the 2, 10 and 20 μg/kg spiked samples ranged from 60.1% to 96.2%, with RSDs of 1.44%~11.1%. Compared with the existing national standard, this new method has the advantage of detecting more types of quinolone drugs, especially the new ones. The new method has a certain reference value for a more comprehensive screening and identification of quinolone residues in eggs and prevention of illegal additions.
