Simultaneous Determination of 15 Quinolones and Tetracyclines Antibiotics in Chicken Gizzard and Liver by QuEChERS-High Performance Liquid Chromatography-Mass Spectrometry
WANG Zhiyu, ZHANG Guifang, ZHANG Xiaoyu, ZHANG Yi, ZHANG Tiantian
Yantai Center for Disease Control and Prevention, Yantai 264003, China
Abstract:A method which can simultaneously determine the residues of 11 quinolones and 4 tetracyclines antibiotics in chicken gizzard and liver was established using high performance liquid chromatography-mass spectrometry (HPLC-MS). The samples were pretreated by the widely used QuEChERS (quick, easy, cheap, effective, rugged, safe) method and extracted with glacial acetic acid-acetonitrile-water (1:84:15, V/V), and then extract was cleaned up using Discovery? DSC-18 sorbent, separated using methanol as mobile phase A and 0.1% formic acid in water as mobile phase B by gradient elution, and detected in the multiple reaction monitoring (MRM) mode. There were good linear relationships between the concentrations of the 15 antibiotics in the range of 2–80 ng/mL and their response values (R2 ≥ 0.993 3). The detection limits of this method were 0.5–3.0 μg/kg and the quantitation limits were 1.7–10.0 μg/kg. The average recovery of spiked samples was 75.2%–104.4% with relative standard deviation (RSD) of 2.7% to 8.7%. When 51 chicken gizzard samples and 49 chicken liver samples were randomly chosen and tested by this method, the total detection rate of the 15 antibiotics was 21.38% and their residual levels were 3.48–154.00 μg/kg.