QuEChERS-超高效液相色谱-串联质谱法同时测定淡水鱼和淡水虾中的11种喹诺酮类兽药残留量

Simultaneous determination of 11 quinolone residues in fresh water fish and shrimp by QuEChERS purification coupled with ultra performance liquid chromatography-tandem mass spectrometry

目的建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定淡水鱼和淡水虾中11种喹诺酮类兽药残留的分析方法。方法样品中的喹诺酮残留经酸化乙腈提取,C18基质分散固相萃取净化,超高效液相色谱-串联质谱测定其中11种喹诺酮类兽药残留量。结果恶喹酸在1~50.0μg/L,其余10种喹诺酮类化合物在1~100.0μg/L范围内线性关系良好,11种喹诺酮药物的检出限为0.5~1.0μg/kg,定量限为1.5~3.0μg/kg,精密度<12%,低、中、高3个浓度加标回收率为70.0%~120.1%。结论该方法样品前处理简单、重现性好、灵敏度高,能满足限量标准的要求,可用于淡水鱼和淡水虾样品中喹诺酮类药物残留的分析检测。

Objective To establish a method for the simultaneous determination of 11 quinolone residues in fresh water fish and shrimp sample by QuEChERS purification combined with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods The target 11 quinolone residues were extracted by acidic acetonitrile and purified by C18 substrate dispersed solid extraction, finally determined by UPLC-MS/MS. Results The method showed good linear relationship within the concentration range of 1.0-50.0 μg/L for oxolinic acid and 1-100.0 μg/L for the other 10 quinolones. The recoveries of 11 quinolone residues ranged from 70.0% to 120.1% with the relative standard deviation less than 12%. The limits of detection and quantitation of 11 quinolone residues were in the range of 0.5-1.0 μg/kg and 1.5-3.0 μg/kg, respectively. Conclusion This method is simple, reproducible and sensitive, and can meet the requirements of the limit standard. It can be used for the determination of quinolones residues in freshwater fish and shrimp samples.