QuEChERS-超高效液相色谱-串联质谱法同时快速测定肉类食品中多种抗生素残留

Rapid determination of 28 antibiotic residues in meat by Qu ECh ERS ultra performance liquid chromatography-tandem mass spectrometry

目的建立能同时检测肉类食品中20种磺胺和8种喹诺酮类抗生素残留的Qu ECh ERS-超高效液相色谱-串联质谱法（UPLC-MS/MS）。方法样品加1%甲酸乙腈提取,经分散固相萃取净化后,采用Waters C18（2.1 mm×100 mm,1.7μm）色谱柱分离,梯度洗脱,采用电喷雾-正离子多反应监测模式,外标法定量。结果 28种抗生素在各自浓度范围内线性关系良好,相关系数（r）为0.997 5-0.999 6,检出限（LOD）为0.17-0.91μg/kg（S/N=3）,磺胺类抗生素回收率在70.9%-115.2%之间,RSD在2.8%-15.9%（n=6）之间;喹诺酮类抗生素回收率在71.3%-112.3%之间,RSD在2.5%-14.6%（n=6）之间。结论建立的方法准确、快速、灵敏度高,可对动物源性食品中多种抗生素残留进行快速分析。

Objective A method was developed for the simultaneous determination of 20 sulfonamides and 8 quinolones antibiotic residues in meat by Qu ECh ERS and ultra performance liquid chromatography-tandem mass spectrometry（ UPLCMS / MS）. Methods The analytes were extracted with 1% formic acid acetonitrile and cleaned up with dispersive-solid phase extraction. The target analytes were separated by Waters C_（18） column with gradient elution. The analytes were detected by tandem quadrupole mass spectrometry after positive electrospray ionization by multiple reaction monitoring（ MRM）. External standard method was used to determine the results. Results The correlation coefficients of 28 antibiotics ranged from 0. 997 5 to 0. 999 6 in the linear range. The limits of detection were 0. 17-0. 91 μg / kg（ S / N = 3）.The recoveries of sulfonamides and quinolones were 70. 9% to 115. 2% and 71. 3%-112. 3% respectively. The RSDs of sulfonamides and quinolones were 2. 8%-15. 9% and 2. 5%-14. 6%（ n = 6）. Conclusion The method was effective,rapid,sensitive,and suitable for the monitoring of multi-antibiotic residues in animal derived foods.