QuEChERS-超高效液相色谱-串联质谱法同时测定畜禽肉中11 种喹诺酮类兽药残留

建立一种超高效液相色谱-串联质谱法测定畜禽肉中恩诺沙星、环丙沙星、氧氟沙星、培氟沙星、诺氟沙星、洛美沙星、沙拉沙星、双氟沙星、司帕沙星、氟罗沙星和达氟沙星共11 种喹诺酮类兽药残留的检测方法。畜禽肉样品经2%甲酸-乙腈均质提取，离心沉淀后上清液经QuEChERS净化剂净化后，经快速溶剂蒸发系统浓缩，采用Waters BEH C18色谱柱（2.1 mm×50 mm，1.7 μm）分离，以0.1%甲酸-水和0.1%甲酸-乙腈为流动相进行梯度洗脱，电喷雾离子源电离，多反应监测模式采集信号，内标法定量。结果表明：11 种喹诺酮类兽药在2～80 ng/mL质量浓度范围内线性关系良好（R2＞0.99），方法的检出限和定量限分别为0.5～2.0 μg/kg和1.5～6.0 μg/kg；空白样品加标量为10、25、50 μg/kg 3 个水平时，11 种喹诺酮类兽药的平均加标回收率为74.52%～106.83%，相对标准偏差为1.8%～8.7%（n=6）。该方法检测过程简单快捷、准确度好、灵敏度高，适用于畜禽肉中喹诺酮类兽药残留的检测。

Simultaneous Determination of 11 Quinolone Residues in Livestock and Poultry Meat by QuEChERS and Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

A method for simultaneous determination of enrofloxacin,ciprofloxacin,ofloxacin,pefloxacin,norfloxacin,lomefloxacin,sarafloxacin,difloxacin,sparfloxacin,flerofloxacin and danofloxacin residues in livestock and poultry meat by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established.Samples were homogenized and extracted with 2%formic acid-acetonitrile.After centrifugation,the supernatant was purified by the QuEChERS procedure,concentrated by a rapid solvent evaporation system,separated on a Waters BEH C18 column(2.1 mm×50 mm,1.7μm)with a mobile phase consisting of 0.1%formic acid-water and 0.1%formic acid-acetonitrile by gradient elution,detected in the multiple reaction monitoring(MRM)mode using an electrospray ionization source(ESI+)and quantified by an internal standard method.The results showed that good linearity was observed for all analytes in the concentration range of 2.0–80.0 ng/mL with correlation coefficients greater than 0.99 and the detection and quantitation limits were respectively 0.5–2.0 and 1.5–6.0μg/kg.The average recoveries of blank samples spiked at 10,25 and 50μg/kg were 74.52%–106.83%,with relative standard deviation(RSD)values of 1.8%–8.7%(n=6).This method proved to be simple,accurate,highly sensitive and suitable for the simultaneous determination of quinolone residues in livestock and poultry meat.