稳定同位素内标-超高压液相色谱-串联质谱法同时测定动物源性食品中8种抗生素残留

Simultaneous determination of eight antibiotics residues in animal food by ultra pressure liquid chromatography-tandem mass spectrometry with stable isotope-labelled internal standards

目的建立超高压液相色谱-串联质谱法（UPLC-MS/MS）测定动物源性食品中8种抗生素药物残留的方法。方法待测物经乙酸乙酯提取,采用电喷雾电离,正负离子扫描,多反应监测模式（MRM）,基质匹配内标标准曲线法定量。结果在最佳试验条件下,8种抗生素残留物在0.05-50.0μg/kg的浓度范围内线性良好,相关系数r2均大于0.995,检出限范围为0.05-0.1μg/kg,平均回收率为56.8%-108.2%,相对标准偏差（RSD）小于15.4%。结论本方法的样品前处理过程简单,净化效果好,灵敏度高,有效解决了基质效应问题,适用于大批量食品中抗生素残留的快速定量分析。

Objective A method for the determination of eight antibiotic residues in animal food by the ultra pressure liquid chromatography-tandem mass spectrometry（ UPLC-MS / MS） was established. Methods The analytes were extracted by ethyl acetate,and the identification was achieved by electrospray ionization in positive and negative mode（ ESI＋ / ESI-） using multiple reaction monitoring（ MRM）. The quantifications were performed by the matrix matched internal standards. Results Under the optimum experimental conditions,the calibration curves of the eight analytes showed a good linearity in the concentrations of 0. 05-50. 0 μg / kg with r-2 above 0. 995. Recoveries were between 56. 8% and 108. 2%with RSD less than 15. 4%. The limits of detection were 0. 05-0. 1 μg / kg. Conclusion The method had the advantages of simple pretreatment, high sensitivity, and lower matrix effects, which was suitable for rapid, high-throughput quantitative food analysis.