同位素稀释-液相色谱-串联质谱法同时测定水产品中13种镇静剂残留  

Simultaneous determination of 13 kinds of sedative residues in aquatic products by isotope dilution-liquid chromatography-tandem mass spectrometry

作　　者：杨洪生[1] 张秋云 谭秀慧[1] 郑伟[2] 朱晓华[1] 陈慧敏 沈美芳[1] YANG Hong-Sheng;ZHANG Qiu-Yun;TAN Xiu-Hui;ZHENG Wei;ZHU Xiao-Hua;CHEN Hui-Min;SHEN Mei-Fang(Freshwater Fishery Research Institute of Jiangsu Province,Nanjing 210017,China;Jiangsu Product Quality Testing and Inspection Institute,Nanjing 210007,China;Shanghai AB Sciex Analytical Instrument Trading Co.,Ltd.,Shanghai 200335,China)

机构地区：[1]江苏省淡水水产研究所,南京210017 [2]江苏省产品质量监督检验研究院,南京210007 [3]上海爱博才思分析仪器贸易有限公司,上海200335

出　　处：《食品安全质量检测学报》2021年第15期6017-6025,共9页Journal of Food Safety and Quality

基　　金：江苏现代农业产业技术体系建设项目(JATS[2020]329);江苏省农业科技自主创新资金项目(CX(19)3008);江苏省“333高层次人才培养工程”项目(BRA2019093)。

摘　　要：目的建立同位素稀释-液相色谱-串联质谱法同时测定水产品中13种镇静剂残留的方法。方法样品采用乙腈-1%氨水溶液提取,提取液经固相萃取柱(Oasis PRIME HLB柱)净化,浓缩后用流动相定容。以1%甲酸水溶液和乙腈为流动相,采用 Agilent InfiniityLab Poroshell 120 SB-C18 色谱柱(2.1 mm×l00 mm,2.7 μm)分离后,在多反应监测(multiple reaction monitoring,MRM)模式下测定,内标法定量。结果 13种镇静剂在0.2-50 μg/L浓度范围内线性关系良好(r>0.99),检出限和定量限分别为0.1-0.2 μg/kg和0.3-0.5 μg/kg。在3个浓度加标水平下的平均回收率为84.0%-116.6%,相对标准偏差为2.1%-9.9%。结论该方法前处理简单、结果准确,适用于水产品种13种镇静剂残留的快速检测。Objective To establish a method for the simultaneous determination of 13 kinds of sedative residues in aquatic products by isotope dilution-liquid chromatography-tandem mass spectrometry(LC-MS/MS). Methods The samples were extracted with acetonitrile-1% ammonia solution. The extract was purified by solid phase extraction column(Oasis PRIME HLB column), and diluted with mobile phase after concentration, then separated by Agilent InfiniityLab Poroshell 120 SB-C18 column(2.1 mm×100 mm, 2.7 μm) using 1% formic acid and acetonitrile as mobile phase, determined in multiple reaction monitoring(MRM) mode and quantified by internal standard method. Results The 13 kinds of sedatives had a good linear relationship within the concentration range of 0.2-50 μg/L(r>0.99). The limits of detection and limits of quantitation were 0.1-0.2 μg/kg and 0.3-0.5 μg/kg, respectively. Average recoveries for the analytes at 3 spiked levels ranged from 84.0% to 116.6% with relative standard deviations(RSDs) of 2.1%-9.9%. Conclusion The method has simple pretreatment and accurate results, and is suitable for the rapid detection of 13 sedative residues in aquatic products.

关 键 词：同位素稀释 液相色谱-串联质谱法 水产品 镇静剂 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]