UPLC-Q/Orbitrap MS法检测水产品中12种抗生素残留  

Determination of 12 Kinds of Antibiotics in Aquatic Products by UPLC-Q/Orbitrap MS

作　　者：李涛 谭璐[2] 徐文泱 杨滔 王芳斌 LI Tao;TAN Lu;XU Wenyang;YANG Tao;WANG Fangbin(Hunan Provincial Food Quality Supervision and Inspection Institute,Hunan Provincial Key Laboratory of Food Safety Monitoring and Early Warning,Changsha 410111;Changsha Commerce&Tourism College,Changsha 410004)

机构地区：[1]湖南省食品质量监督检验研究院,食品安全监测与预警湖南省重点实验室,长沙410111 [2]长沙商贸旅游职业技术学院,长沙410004

出　　处：《食品工业》2020年第5期300-303,共4页The Food Industry

基　　金：湖南省食品药品监督管理局食品药品安全科技项目(编号:湘食药科R201814);湖南省科技厅项目(湘科计(2019)56号),创新平台编号:2019TP1058。

摘　　要：试验旨在采用超高效液相色谱-四极杆/轨道阱高分辨质谱(UPLC-Q/Orbitrap MS)建立水产品中7种大环内酯类和5种四环素类抗生素类药物的快速检测方法。样品采用80%乙腈Na2EDTA-Mc Ilvaine溶液提取, Hypersil Gold C18色谱柱(150 mm×2.1 mm, 3μm)分离,使用0.1%甲酸水溶液和乙腈进行梯度洗脱,流速0.2 mL/min,柱温30℃,正离子模式扫描。结果表明, 12种抗生素在2.0~50.0 ng/mL范围内具有良好的线性关系(R2>0.996),各组分检出限在0.073~17μg/kg之间,定量限在0.24~55μg/kg之间。回收率在83.1%~95.7%之间,精密度在0.8%~5.6%之间。该方法简单高效、灵敏度高,为水产品中大环内酯类和四环素类抗生素检测提供方法参考。A rapid method was presented for the determination of 12 macrolides antibiotics and tetracycline antibiotic in aquatic products by ultra-performance liquid chromatography-quadrupole orbitrap high resolution mass spectrometry. The samples were extracted with 80% acetonitrile Na2EDTA-Mc Ilvaine, and separated by Hypersil Gold(150 mm×2.1 mm, 3 μm) using a binary solvent system composed of acetonitrile and water(0.1% formic acid) at a flow rate of 0.2 mL/min, and the column temperature was 30 ℃. The positive mode was used in the MS detection. The results indicated that the linearity of all the 12 antibiotics ranged from 2.0 ng/mL to 50.0 ng/mL with the correlation coefficients greater than 0.996. The LOD was in the range of 0.073-17 μg/kg and the LOQ was in the range of 0.24-55 μg/kg. The recoveries were in the range of 83.1% to 95.7%, with the precision in the range of 0.8%-5.6%. The method was simple, rapid and accurate, and it provided a reference for the determination of macrolide and tetracycline antibiotics in aquatic products.

关 键 词：四极杆/静电场轨道阱高分辨质谱 大环内酯类 四环素 水产品 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]