超高效液相色谱串联质谱法测定鳗鱼中大环内酯类和林可酰胺类抗生素残留量的研究

本文建立了鳗鱼中9种大环内酯类和林可酰胺类药物残留量的超高效液相色谱-串联质谱同时测定的方法。采用中性磷酸盐缓冲液水解,乙腈萃取,正己烷脱脂,固相萃取小柱净化,电喷雾串联质谱进行检测,多离子反应监测(MRM)模式,外标法定量。在0～100μg/L内,峰面积与质量浓度有良好的线性关系,相关系数大于0.9900,在1.0、2.0、4.0μg/kg3个浓度水平进行验证试验,总体平均回收率为70.26%～124.22%,相对标准偏差为1.31%～16.00%,各项技术指标均满足国内外法规要求。结果表明:该法快速、高效、特异性强,可用于鳗鱼样品中大环内酯类及林可酰胺类抗生素残留量的确证检测。

Study on Determination of Residues of Macrolides and Lincosamides Antibiotics in Eel by Ultra-performance Liquid Chromatography-Electrospray Tandem Mass Spectrometry

An ultra-performance liquid chromatographic method with tandem mass-spectrometric detection was developed for the simultaneous analysis of 9 macrolide and lincosamides antibiotics in eel. The samples were firstly dispersion with phosphate buffer buffer solutions; The target compounds were extracted with acetonitrile,and then cleaned up with solid phase extraction cartridges,followed by liquid chromatography-tandem mass spectrometry analysis. The range linearity was from 0 to 100μg/L and the linear correlation coefficient was more than 0.9900. The method was validated at 1.0,2.0 and 4.0μg/kg. The validation results were as follows： the average recovery for all the compounds was 70.26%～124.22%,variation coefficients was 1.31%～ 16.00%.The results showed that the established method was fast,effective,specific and quite suitable for identification and quantity of macrolide and lincosamides antibiotics in eel.