改进的QuEChERS结合超高效液相色谱—串联质谱法同时测定水产品中19种兽药残留

Modified QuEChERS method combined with ultra-high performance liquid chromatography-tandem mass spectrometry for simultaneous determination of 19 quinolones and sulfonamides in aquatic products

目的:实现水产品中19种磺胺、氟喹诺酮类兽药同步检测。方法:利用1.0%甲酸乙腈溶液作为提取液,超声1 min对样品中目标分析物进行提取,采用QuEChERS多功能针式过滤器净化样品,样品净化与过滤除杂同步进行,采用超高效液相色谱结合三重四极杆质谱进行检测。结果:19种磺胺、喹诺酮类兽药的检出限为0.5~1.0μg/kg,与国家标准方法相比,检测灵敏度有所提高。添加回收率为81.0%~113.0%,相对标准偏差(RSD)为0.2%~11.7%。结论:该方法通过超声辅助萃取、QuEChERS多功能针式过滤器提高样品前处理效率,具有方法检测灵敏度高、准确度高、重现性良好等优点,适用于大批量水产品样品中磺胺、喹诺酮类兽药日常监测。

Objective:A simultaneous determination method was established for detecting 19 kinds of quinolones and sulfonamides in aquatic products simultaneously,by using QuEChERS combined with UPLC-MS/MS.Methods:Samples were extracted with 1.0%formic acid acetonitrile solution,ultrasonic for 1 min,and purified by QuEChERS multi-function needle filter.The sample purification and filtering were performed simultaneously.The Mass spectrometry was conducted by using positive(ESI+)electrospray ionization and multi-reactions monitoring(MRM)models,with external standard method.Results:The detection limit of 19 kinds of sulfonamides and quinolones is from 0.5 to 1.0μg/kg.Compared with the national standard method,the detection sensitivity is improved.The added recoveries were from 81.0%to 113.0%,and the relative standard deviation(RSD)were from 0.2%to 11.7%.Conclusion:This method assisted ultrasonic extraction and QuEChERS,enhanced the efficiency of measuring quinolones and sulfonamides in aquatic products.It is a simple,rapid,sensitivity,accurate method,which provides an efficient technical means for daily monitoring of sulfonamides and quinolones in large quantities of aquatic product samples.