基质固相分散-液相色谱-串联质谱联用技术检测鸡蛋中14种氟喹诺酮类药物残留

Matrix Solid-Phase Dispersion Coupled with Liquid Chromatography-Tandem Mass Spectrometry for the Determination of Fluoroquinolones Residues in Eggs

本工作建立了一种基质固相分散-液相色谱-串联质谱(LC-MS/MS)联用技术测定鸡蛋中14种氟喹诺酮类药物残留的新方法。基质固相分散提取过程中以硅胶为分散剂,氨甲醇溶剂为洗脱剂,其萃取回收率在80%以上。洗脱液浓缩定容后经Shimpack GISS C_(18)柱(50×2.1mm,1.9μm)分离,质谱采用电喷雾电离、正离子模式(ESI+),以多反应监测(MRM)模式进行检测。方法的线性范围为0.1~50μg/kg,检出限达到0.1μg/kg,相对标准偏差为8.8%~10.4%。方法检出限优于国家标准方法,可满足实际样品分析的要求。

A new method of matrix solid-phase dispersion coupled with liquid chromatography-tandem mass spectrometry was developed for the determination of fourteen kinds of fluoroquinolones residues in eggs.With silica gel as a dispersant and ammonia methanol as eluent,the recoveries of fluoroquinolones in matrix solid-phase dispersion extraction were higher than 80%.The elution solution was then concentrated and introduced into a C_（18） column for chromatographic separation.The identification and quantification of target analytes were performed using electrospray ionization in positive mode and multiple reaction monitoring（MRM）.Under the optimized condition,the linear ranges were 0.1-50μg/kg with the RSDs of 8.8%-10.4%,and the limits of detection were 0.1μg/kg,which were lower than the values required by National Standards of China.