通过式固相萃取结合高效液相色谱-四极杆飞行时间质谱测定鸡蛋中62种兽药残留

Determination of 62 Veterinary Drug Residues in Eggs by Solid-phase Extraction Combined with High-performance Liquid Chromatography Quadrupole Time of Flight Mass Spectrometry

建立了固相萃取结合高效液相色谱-四极杆飞行时间质谱(HPLC-QTOF)同时测定鸡蛋中62种兽药残留的方法。鸡蛋均质后经90%甲酸乙腈水溶液提取后,PRiME HLB固相萃取小柱净化,氮吹后复溶,用(HPLC-QTOF)进行检测。62种兽药在0.5~500 ng/mL浓度范围内线性关系良好(r^(2)≥0.99),回收率在71.2%~113%之间,日内变异系数范围为1.3%~14.3%,日间变异系数范围为4.2%~18.3%,检测限为1.0~2.0μg/kg,定量限为2.0~5.0μg/kg。本方法简便快捷、准确可靠,适用于鸡蛋中62种兽药的同时测定。

A method was established for the simultaneous determination of 62 veterinary drug residues in eggs using solid-phase extraction combined with high-performance liquid chromatography quadrupole time of flight mass spectrometry(HPLC-QTOF).The homogenizing eggs were extracted with a 90%formic acid acetonitrile aqueous solution,purified with PRiME HLB solid-phase extraction column,and dissolved again after nitrogen blowing and detected by HPLC-QTOF.62 veterinary drugs have good linear relationships(r^(2)≥0.99)within the concentration range of 0.5~500 ng/mL with recoveries ranging from 71.2%to 113%,intraday variation coefficients ranging from 1.3 to 14.3%,intraday variation coefficients ranging from 4.2 to 18.3%,and the detection limit was 1.0~2.0μg/kg,limit of quantitation was 2.0~5.0μg/kg.This method is simple,fast,accurate,reliable and suitable for the simultaneous determination of 62 veterinary drugs in eggs.