高效液相色谱串联质谱法测定饲料中喹烯酮含量

DETERMINATION OF QUINOCETONE IN ANIMAL FEED SAMPLES BY HIGH PERFORMANCE LIQUID CHROMATORGRAPHY - TANDEM MASS SPECTROMETRY

建立了液相色谱串联质谱法(HPLC/MS/MS)测定饲料中喹烯酮的含量的方法。饲料样品经匀浆、超声提取后经固相萃取柱[中性氧化铝Alumia N(1 g,3 mL)]净化,采用HPLC/MS/MS电喷雾电离,正离子模式,多反应监测(MRM)。喹烯酮浓度在0.01～0.2μg/g范围内标准曲线的相关系数大于0.998。在不同添加水平下的回收率为81.9%～111.6%,检出限(LOD)为5μg/kg。

A high performance liquid chromatography - tandem mass spectrometry method was established for determination of quinotone in animal feed. Animal feed samples were extracted by a homogenater and an ultrasonic cleaner, purified by a solidphase extraction （SPE） cartridges [ Alumia N （1 g, 3 mL） ] , detected by the positive eleetrospray ionization （ESI ＋ ） method under muhiple reaction monitoring （MRM） mode. The calibration curves were liner （r 〉 0. 998 ） in the concentration range of 0.01- 0.2 μg/g. The extraction recoveries range from 81.9% to 111.6% in different spiked concentrations samples. The LOD was 5 μg/kg.