超高压液相色谱-串联质谱法测定肉类中沃尼妙林和泰妙菌素的残留量  

Determination of Valnemulin and Tiamulin Residues in Meat Using Liquid Chromatography-Tandem Mass Spectrometry

作　　者：刘晓茂[1] 李学民[1] 葛娜[1] 王飞[1] 杨志伟[1] 曹彦忠[1] 

机构地区：[1]秦皇岛出入境检验检疫局,河北秦皇岛066004

出　　处：《食品与发酵工业》2012年第8期182-186,共5页Food and Fermentation Industries

摘　　要：建立了固相萃取-高效液相色谱-串联质谱(UPLC-MS/MS)测定肉类中沃尼妙林和泰妙菌素残留量的分析方法。样品用乙腈提取,OasisMCX SPE小柱净化,经C18色谱柱分离,以电喷雾离子源(ESI)在正离子多反应监测(MRM)模式下进行测定,外标法定量。沃尼妙林和泰妙菌素的检出限均为0.04μg/kg,定量下限均为0.1μg/kg,在0.1～50.0μg/L内线性关系良好,相关系数r均大于0.99。在0.1～10.0μg/kg的加标水平内的回收率为80%～94%,RSD为4.5%～8.2%。该方法实用、准确、灵敏,适用于肉类中沃尼妙林和泰妙菌素残留量的测定。A method was developed for the determination of valnemulin and tiamulin residues in meat by solid- phase extraction clean up-liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）. The sample was extrac- ted by acetonitrile, purified by solid phase extraction （SPE） with oasis MCX extraction catridge. C18 column was the separation column, positive eleetrospray ionization was performed under multiple reaction monitoring （MRM） mode. The limit of detection for valnemulin and tiamulin was 0. 04μg/kg, and the limit of quantization was 0.1 μg/kg. The calibration curve showed a good linear from 0.1 μg/kg to 50.0μg/kg with a correlation coefficient of 0.99. The recoveries of valnemulin and tiamulin at spiked levels in the range of 0.1 - 10.0μg/kg were 80% - 94% with relative standard deviations of 4.5% -8.2%. The method was practical, accurate and sensitive, and was suitable for the determination of valnemulin and tiamulin residues in meat.

关 键 词：超高压液相色谱-串联质谱 固相萃取净化 沃尼妙林 泰妙菌素 残留 

分 类 号：S859.84[农业科学—临床兽医学]