增强型脂质去除净化剂结合液质联用法同时测定水产和畜禽产品中氟喹诺酮和磺胺类药物残留  

Determination of quinolones and sulfonamides residues in aquatic products and livestock products with enhanced matrix removal-lipid adsorbent by liquid chromatography-tandem mass spectrometry

作　　者：秦宇 薛峰[2] 俞君杰[2] 刘洋 宫衡 QIN Yu;XUE Feng;YU Junjie;LIU Yang;GONG Heng(School of Biotechnology,East China University of Science and Technology,Shanghai 200237,China;Shanghai Institute of Quality Inspection and Technical Research,Shanghai 200233,China)

机构地区：[1]华东理工大学生物工程学院,上海200237 [2]上海市质量监督检验技术研究院,上海200233

出　　处：《食品与机械》2025年第1期63-73,共11页Food and Machinery

基　　金：国家市场监督管理总局科技计划项目(编号:2023MK034)。

摘　　要：[目的]实现水产和畜禽产品中喹诺酮类(QNs)和磺胺类(SAs)残留的同时测定。[方法]前处理比较了提取溶剂对回收率的影响,考察了EMR-Lipid与液液萃取(正己烷)、基质分散吸附(C_(18)和乙二胺-N-丙基硅烷化硅胶)和通用型固相萃取(PRiME HLB)等净化方式对基质效应减弱或消除的效果。以1.0%甲酸—乙腈为提取溶剂,通过EMR-Lipid净化;采用ACQUITY UPLC■HSS T_(3)柱(3.5μm,2.1 mm×100 mm)在10 min内完成分离;质谱采用正离子扫描和多反应监测模式下监测,外标法定量。[结果]该方法的线性范围为1.0~100.0 ng/mL,相关系数(R2)均大于0.99;检出限和定量限分别为1.0,2.0μg/kg;低、中、高加标回收率为61.9%~115.3%,相对标准偏差<15%。[结论]与文献和标准方法相比,该方法拓宽了适用范围,减少了前处理流程,降低了方法使用时间和经济成本。[Objective]To establish a new method for simultaneous detection of quinolones(QNs)and sulfonamides(SAs)in aquatic products and livestock products.[Methods]In pretreatment,this work compares the effect of extraction solvents on the recoveries and investigates the reduction or elimination effect of purification methods such as liquid-liquid extraction(n-hexane),dispersive adsorption of the matrix(C_(18)and ethylenediamine-N-propyl silylated silica),and general solid phase extraction(PRiME HLB)on the matrix effect.The sample is pretreated by acetonitrile with 1.0%formic acid,purified by EMR-Lipid,and separated by ACQUITY UPLC®HSST_(3)column(3.5μm,2.1 mm×100 mm)in 10 min.MS detection is performed by multi-reaction monitoring(MRM)in positive ion mode.QNs and SAs are quantified by the external standard method.[Results]The calibration curves of QNs and SAs exhibit a good linear relationship with the correlation coefficients(R2)exceeding 0.99,in the range of 1.0~100.0 ng/mL.The limits of detection(LODs)and quantification(LOQs)are 1.0 and 2.0μg/kg,respectively.The average recoveries of QNs and SAs are between 61.9%and 115.3%under low,middle,and high spiked levels and the relative standard deviations(RSDs)are less than 15%(n=6).[Conclusion]Compared with literature and standard methods,the established method increases the scope of application and reduces the pre-treatment process and cost.

关 键 词：增强型脂质去除净化剂 液相色谱串联质谱法 喹诺酮 磺胺 水产品 畜禽产品 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学] TS251.7[轻工技术与工程—水产品加工及贮藏工程]