分子印迹固相萃取-超高效液相色谱-串联质谱法测定鸡肉中9种氟喹诺酮药物残留

建立了分子印迹固相萃取（MISPE）-超高效液相色谱-串联质谱（UPLC-MS/MS）同时测定鸡肉中9种氟喹诺酮药物残留的分析方法。样品经均质处理后，采用磷酸盐缓冲液提取，提取液经MISPE柱净化后，采用BEH C₁₈柱分离，以乙腈-0.1%（v/v）甲酸水溶液为流动相，梯度洗脱，采用电喷雾正离子多反应监测模式，外标法定量。考察了MISPE柱对9种氟喹诺酮药物的吸附特异性；9种药物在0.25~100 μg/L范围内线性关系良好，相关系数（r）>0.9965；检出限和定量限分别为0.08 μg/kg和0.25 μg/kg；在0.25、2.5、5.0 μg/kg添加水平下，9种药物的回收率为65.8%~112.2%，批内、批间RSD分别为0.6%~13.5%和0.5%~14.9%；MISPE的最大柱容量为464.7~932.4 μg/L。该方法灵敏度好、操作简单、快速。

Determination of nine fluoroquinolone residues in chicken by ultra performance liquid chromatography-tandem mass spectrometry coupled with molecularly imprinted solid phase extraction

An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method coupled with molecularly imprinted solid phase extraction (MISPE) for the determination of nine fluoroquinolone residues in chicken was developed. The samples were extracted with phosphate buffer solution, and cleaned up with MISPE columns. Then the drugs were analyzed on a BEH C₁₈ column by gradient elution with acetonitrile and 0.1% (v/v) formic acid solution as mobile phase. The samples were analyzed in electrospray positive ion mode and multiple reaction monitoring (MRM) mode. The analytes were quantified by external standard method. The specific adsorption of MISPE for the nine fluoroquinolones in chicken samples was investigated. The linear ranges were 0.25-100 μg/L with correlation coefficients (r) greater than 0.9965. The limits of detection (LODs, S/N=3) and the limits of quantification (LOQs, S/N=10) were 0.08 μg/kg and 0.25 μg/kg, respectively. At the spiked levels of 0.25, 2.5, 5.0 μg/kg, the recoveries were 65.8%-112.2% with the intra-RSDs of 0.6%-13.5% and inter-RSDs of 0.5%-14.9%, respectively. The maximum capacities of the MISPE column were 464.7-932.4 μg/L. The method is sensitive, simple and rapid for the simultaneous determination of the nine fluoroquinolone residues.