超高压液相色谱-电喷雾串联四极杆质谱内标法同时测定禽类食品中11种喹诺酮类药物

Simultaneous determination of eleven quinolones drug residues in poultry products by ultra performance liquid chromatography-electrospray ionization tandem quadrupole mass spectrometry with isotope-labelled internal standards

目的建立同时测定禽类食品中11种喹诺酮类药物残留量的超高压液相色谱-电喷雾串联四极杆质谱(UPLC-ESI-MS/MS)分析方法。方法鸡肉和鸡蛋样品经1%乙酸乙腈(1∶100,V/V)混合液提取,冷冻离心与正己烷脱脂净化,以10 mmol/L乙酸铵(含0.1%甲酸)-甲醇为流动相,采用电喷雾电离,正离子扫描,多离子反应监测(MRM)模式,基质匹配同位素内标,标准曲线法定量。结果 11种喹诺酮类药物在0.05~50.0μg/L的浓度范围内线性良好,相关系数R^2≥0.997 4,检出限范围为0.05~0.10μg/kg,平均回收率为82.4%~104.3%,相对标准偏差小于15.0%。结论该方法的样品前处理过程简单,净化效果好,减少了基质效应的影响,适用于大批量禽类食品中喹诺酮类药物残留量的快速测定。

Objective A method for the determination of eleven quinolones drug residues in chicken and egg by the ultra performance liquid chromatography-electrospray ionization tandem quadrupole mass spectrometry（ UPLC-ESI-MS/MS） was established. Methods The analytes in chicken and egg were extracted by 1% acetic acid-acetonitrile,and the fat were separated by centrifugation and extraction using hexane. The eleven analytes were separated by the mobile phase of10 mmol/L ammonium acetate（ contain 0. 1% formic acid）-methanol on gradient elution. The identifications were achieved by electrospray ionization in positive mode（ ESI ＋） using multiple reaction monitoring（ MRM）. The quantifications were performed by the matrix matched isotope-labelled internal standards. Results The calibration curves of the eleven analytes showed a good linearity in the range of 0. 05-50. 0 μg/L with R^2 above 0. 997 4. Recoveries were between 82. 4% and 104. 3% with RSD less than 15. 0%. The limits of detection were 0. 05-0. 10 μg/kg. Conclusion The method had the advantages of simple pretreatment and low matrix effects,which was suitable for the rapid,highthroughput quantitative analysis of quinolones drug residues in poultry food.