固相萃取-高效液相色谱/串联质谱法测定水产品中硫酸新霉素残留量  

Determination of Neomycin Sulfate in Aquatic Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry with Solid Phase Extraction

作　　者：刘永涛[1,2] 李乐[3] 徐春娟[1,4] 胥宁[1,2] 董靖[1,2] 杨秋红[1] 杨移斌[1] 艾晓辉[1,2] LIU Yong-tao LI Le XU Chun-juan XU Ning DONG Jing YANG Qiu-hong YANG Yi-bin AI Xiao-hui(Yangtze River Fisheries Research Institute,Chinese Academy of Fishery Sciences ,Wuhan 430223 Hubei Freshwater Aquaculture Collaborative Innovation Center ,Wuhan 43022 Chinese Academy of Fishery Sciences ,Beijing 100141 College of Fisheries and Life Science, Shanghai Ocean University, Shanghai 201306)

机构地区：[1]中国水产科学研究院长江水产研究所,湖北武汉430223 [2]淡水水产健康养殖湖北省协同创新中心,湖北武汉430223 [3]中国水产科学研究院,北京100141 [4]上海海洋大学水产与生命学院,上海201306

出　　处：《分析科学学报》2017年第1期6-10,共5页Journal of Analytical Science

基　　金：公益性行业(农业)科研专项(No.201203085;201503108)

摘　　要：建立了一种分析水产品中硫酸新霉素残留量的固相萃取-高效液相色谱/串联质谱法。样品经三氯乙酸水溶液提取,固相萃取小柱净化。用带加热电喷雾离子源的高效液相色谱/串联质谱以选择反应离子监测(SRM)正离子模式检测,基质标准曲线定量。结果显示,在草鱼、斑点叉尾鮰、鳗鲡、南美白对虾和甲鱼空白肌肉中添加硫酸新霉素水平为25~1 000μg/kg时,其加标回收率为91.04%~114.57%,相对标准偏差为1.91%~9.62%。硫酸新霉素的检测限为10μg/kg,定量限为25μg/kg。方法适用于水产品中硫酸新霉素残留量的测定,也适用于硫酸新霉素在水产动物体内组织分布和消除研究。An effective method was developed for the determination of neomycin sulfate residue in aquatic products by high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）.The samples were extracted with trichloroacetic acid-water solution,cleaned up using Waters Oasis HLB solid phase extraction column and detected by a selective reaction monitoring（SRM）mode with positive heated electrospray ionization（HESI）and matrix-matched standard curve for quantification.At the spiked levels of 25-1 000μg/kg,the recoveries were from 91.04%to 114.57%,and the relative standard deviations were from 1.91%to 9.62%.The detection limit for neomycin sulfate was 25μg/kg,and the quantification limit was 50μg/kg.The method is suitable for the determination of neomycin sulfate in aquatic products,tissue distribution and depletion studies in aquatic animals.

关 键 词：水产品 硫酸新霉素 残留 高效液相色谱串联质谱 

分 类 号：O657.63[理学—分析化学]