建立饲料中16种氟喹诺酮类药物残留检测的高效液相色谱-串联质谱分析方法(HPLC-MS/MS).样品经水浸泡1h,1%乙酸的乙腈溶液提取,Oasis MCX固相萃取柱净化,16种氟喹诺酮类药物经色谱柱分离,以乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱,外标峰面积法定量.结果表明,16种氟喹诺酮类药物在5.0 μg/kg ~100.0 μg/kg范围内呈良好的线性关系,3个浓度添加水平的回收率范围为70.7 %~86.4%,相对标准偏差在3.8%~9.2%之间.
A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was established for the determination of 16 quinolones residues in the feed. Samples were soaked in water for 1 hour and extracted by acetonitrile (0.1% acetic acid) solution. Extraction liquid was purified by Oasis MCX SPE column. The separation of 16 quinolones was performed on Cls column. The mobile phases were acetonitrile and water (containing 0.1% formic acid)in gradient elution. External standard method was adopted as the quantitative method. The calibration cuives showed good linearity within the concentrations of 5.0 μg/kg-100.0 μg/kg, and the recoveries were 70.7 %-86.4 % with the correlation coefficients 3.8 %-9.2 %.