石墨烯作为新型固相萃取填料结合UPLC-MS/MS测定黑鱼中13种磺胺类药残

Graphene as a novel SPE adsorbent coupled with UPLC-MS/MS for the determination of sulfanilamide residues in black fish tissues

摘要: 建立了以石墨烯为固相萃取填料,结合高效液相色谱-电喷雾离子阱质谱联用技术测定黑鱼中磺胺类兽药残留的检测方法。采用甲醇作为提取溶剂,经石墨烯固相萃取柱净化富集,质谱采用电喷雾正离子源,多反应监测模式。方法的线性良好,相关系数大于0.998,检出限范围0.048⁰.288μg/kg,定量限为0.160⁰.960μg/kg,线性范围内的加标回收率为70.6%⁹3.8%。本方法灵敏、可靠、稳定,满足复杂水产品基质中磺胺类药残检测的需要。

Abstract: A rapid method for the simultaneous determination of thirteen sulfonamide(SAs) in black fish had been developed. The samples were extracted by Me OH and enriched by solid-phase extraction using a novel material-graphene as the sorbent. Chromatography separation was performed by UPLC and the detection was achieved by tandem mass spectrometry using ESI+and MRM mode. The method had a good linear range and the correlation coefficient was greater than 0.998. The limit of detection(LOD) ranging from 0.048 to 0.288μg/kg and the limit of quantization(LOQ) ranging from 0.160 to 0.960μg/kg were obtained. Average recoveries of individual sulfonamide were btween 70.6% and 93.8%. The proposed method was sensitive,effective and stable,which was satisfied with the need in application of detection of SAs residues in various aqutic matrixes aquatic products.