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

关键词:  鸡蛋  通过式固相萃取  高效液相色谱-四极杆飞行时间质谱  兽药残留

Key words:  Eggs  Solid phase extraction purification  High performance liquid chromatography quadrupole time of flight mass spectrometry  Veterinary drug residues

摘要:

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(r2≥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1.0~2.0 μg/kg，定量限为2.0 ~5.0 μg/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。

Abstract:

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 ≥ 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 1.0~2.0 μg/kg, limit of quantitation was 2.0 ~5.0 μg/kg. This method is simple, fast, accurate, reliable and suitable for the simultaneous determination of 62 veterinary drugs in eggs.