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应用液相色谱-串联质谱法检测饲料中的氟喹诺酮类药物,用含1%甲酸的甲醇提取饲料中的氟喹诺酮类药物,HLB固相萃取柱净化,0.22μm滤膜过滤后用液相色谱-串联质谱法测定,基质匹配标准曲线校正,外标法定量。检测限可达到0.1 mg/kg,定量限可达到0.5 mg/kg,能很好的满足检测要求。各种饲料中氟喹诺酮类药物的平均回收率均可达70%~120%;日内变异系数范围均小于15%,日间变异系数均小于15%,方法回收率高,精密度好。从方法的线性、灵敏度、准确度和精密度等方面进行试验与考察,证明试验方法设计合理,实用有效,检测方法中样品处理相对较简单,所用时间较短,适用于饲料的范围比较广泛。
Fluoroquinolones in feed were detected by liquid chromatography-tandem mass spectrometry. Fluoroquinolones were extracted from feed by methanol containing 1% formic acid. HLB solid-phase extraction cartridge was used to purify. After filtration with 0.22μm membrane, - Tandem mass spectrometry, matrix matching standard curve calibration, external standard method. The detection limit can reach 0.1 mg / kg, the limit of quantification can reach 0.5 mg / kg, which can meet the testing requirements well. The average recoveries of fluoroquinolones in various feedstuffs were up to 70% ~ 120%. The intra-day coefficient of variation was less than 15% and the intra-day coefficient of variation was less than 15%. The recovery rate was high and the precision was good. From the aspects of the linearity, sensitivity, accuracy and precision of the method, it is proved that the test method is reasonable in design, practical and effective. The sample processing in the detection method is relatively simple, the time used is short, and the scope of application is relatively wide.