分散固相萃取剂-液相色谱串联质谱法测定鸡肉和鸡蛋中氟苯尼考和氟苯尼考胺残留

Determination of florfenicol and florfenicol amine residuesin chicken and eggs by HPLC-MS/MS

建立分散固相萃取剂-液相色谱串联质谱法(HPLC-MS/MS)同时检测鸡肉及鸡蛋中氟苯尼考和氟苯尼考胺的方法。样品用乙腈提取,C18分散固相萃取填料净化,乙腈饱和的正己烷脱脂,电喷雾离子源正负模式切换,HPLC-MS/MS多反应监测(MRM),同位素内标法定量。氟苯尼考和氟苯尼考胺线性范围分别为0.1 ng/mL~2.0 ng/mL和1.0 ng/mL~20.0 ng/mL;线性相关系数均大于0.995。该方法检出限氟苯尼考和氟苯尼考胺分别为0.05μg/kg和0.5μg/kg,远低于GB31650—2019限量要求,满足限量判定需要;低、中、高3水平添加回收率在68.0%~90.8%之间,精密度均小于5%。该方法检出限低、准确度高和操作方便,可以高效处理批量样品。

A method for simultaneous determination of florfenicol and florfenicol amine residues in chicken and eggs by dispersed solid phase extractant,liquid chromatography tandem mass spectrometry(HPLC-MS/MS)was established.Samples were extracted with acetonitrile,purified by C18 dispersed solid phase extraction packing,degreased with n-hexane saturated by acetonitrile,switched by positive and negative mode of electrospray ionization source,monitored by HPLC-MS/MS multiple reaction(MRM),and quantitatively determined by isotope external standard method.The linear ranges of florfenicol and florfenicol amide were 0.1 ng/mL~2.0 ng/mL and 1.0 ng/mL~20.0 ng/mL,respectively.The linear correlation coefficients were both more than 0.995.The limit of florfenicol and florfenicol amide detected by this method was 0.05μg/kg and 0.5μg/kg,respectively,which were much lower than the limit requirements of GB 31650—2019 and met the needs of limit determination.The recoveries of low,medium and high levels were 66.0%~90.8%and the precision was all less than 5%.This method had the advantages of low detection limit,high accuracy and convenient operation,and could efficiently deal with batch samples.