超高效液相色谱-串联质谱法测定猪肝中14种喹诺酮类药物残留

Determination of 14 kinds of quinolones residues in pig liver by ultra performance liquid chromatography-tandem mass spectrometry

目的建立猪肝中14种喹诺酮类抗生素残留的提取、净化和超高效液相色谱串联质谱测定的方法。方法样品采用EDTA缓冲溶液提取、经正己烷除脂、固相萃取柱净化后,利用超高效液相色谱串联质谱法检测。结果本方法显著地除去了动物内脏中的磷脂类杂质的干扰,待测物均获得了良好的信号响应。方法回收率为72.7%~116.8%、相对标准偏差(relative standard deviation,RSD)为1.6%~19.5%、定量限均为1.0μg/kg。结论本方法前处理简单、重复性好、定量限低,适合作为猪肝中喹诺酮类抗生素残留的日常检测方法。

Objective To establish an analytical method for extraction, purification and detection of 14 kinds of quinolone residues in pig liver by ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）. Methods Samples were extracted by EDTA buffer, the fat was removed by n-hexane, then purified by solid phase extraction column and detected by ultra performance liquid chromatography tandem mass spectrometry. Results This method significantly removed the interference ofphospholipid impurities in the animal＇s liver, and a good signal response was obtained. The recoveries of the method were 72.7%-116.8%, the relative standard deviations （RSDs） were 1.6%-19.5%, and the limit of quantitation was 1 μg/kg. Conclusion The established method is simple, well repeatable and sensitive, which is suitable for routine detection of quinolones residues in pig liver.