改良QuEChERS-超高效液相色谱-串联质谱同时检测淡水鱼中11种喹诺酮类抗生素残留

Determination of 11-quinolone-antibiotic residues in freshwater fish sold on the market by ultra-high performance liquid chromatography-tandem mass spectrometry with improved QuEChERS pretreament

目的 优化QuEChERS前处理方法,使用超高效液相色谱-串联质谱法检测市售淡水鱼中11种喹诺酮类抗生素残留情况。方法 样品经乙酸乙腈水溶液提取,无水硫酸钠脱水,C18吸附剂净化,基质匹配外标法超高效液相串联质谱测定11种喹诺酮类残留量。结果 11种目标物在5~1 000μg/kg内标准曲线相关系数为0.999 2~0.999 9,检出限范围0.2~1.0μg/kg,定量限范围0.5~3.0μg/kg,平均加标回收率为71.6%~108.8%,相对标准偏差为2.0%~12.6%。结论方法可靠、重现性好、灵敏度高,能满足淡水鱼中多种喹诺酮药物残留的快速定性定量检测要求。

Objective To establish an improved QuEChERS pretreatment method for rapid determination of 11-quinolone-antibiotic residues in freshwater fish sold on the market by ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS).Methods The samples were extracted with acetic acetonitrile aqueous solution,dehydrated with anhydrous sodium sulfate,and purified with C18 adsorbent;the residues of 11 quinolones were determined with matrix-matched external standard by UHPLC-MS/MS.Results The correlation coefficients of the standard curves for the 11 targets within 5-1 000μg/kg were 0.999 2-0.999 9,the limits of detection were 0.2-1.0 μg/kg,the limits of quantitation were 0.5-3.0 μg/kg,the average recoveries were 71.6%-108.8%,and the relative standard deviations(RSD) were 2.0%-12.6%.Conclusion The method is reliable,reproducible and sensitive,which can meet the requirements of rapid qualitative and quantitative determination of quinolone residues in freshwater fish.