液相色谱-电喷雾串联质谱联用检测鳗鱼肌肉组织中4种硝基呋喃类代谢物残留量

Determination of four nitrofuran metabolites in eel muscle by liquid chromatograph-electrospray ionization-mass spectrometry

采用代谢物水解与衍生化同步进行，液液萃取，串联质谱（ESI^＋）MRM检测．外标法定量，成功测定了鳗鱼肌肉组织中4种硝基呋喃类代谢物残留量．标准曲线线性良好．定量定为0．5ng·g^-1检测限为0．25ng·g^-1，在添加浓度0．5～10ng·g^-1范围内，4种代谢物添加回收率为70％～130％。方法快速、简便、经济．符合出口日本、欧盟等国家的检测限量要求（1．0ng·g^-1）。

An external method based on liquid chromatograph-electrospray ionization-mass spectrometry was developed for the determination of low-level residues of four nitrofuran in eel muscle. The procedure entailed an acid-catalyzed release of protein-bound metabolites, followed by the derivation, liquid-liquid extraction, positive electrospray ionization applying multiple reaction and monitoring two transitions for each compound. The standard curve was reliable, the LOQ was 0. 5 ng·g^-1 , the nitrofuran metabolite recovery rates at 5 fortification levels （i. e. , 0. 5, 1.0, 2.0, 5.0, 10. 0 ng·g^-1） were 70% -130%. The LOD was 0. 25 ng·g^-1. The method was rapid, simple economical and its LOQ below the minimum performance limit of 1 ng·g^-1 set by Japan and the EU.