超高效液相色谱-串联质谱法快速检测水产品中喹乙醇及其代谢物3-甲基-喹恶啉-2-羟酸的残留.pdf

现代食品科技 Modern Food Science and Technology 2013, Vol.29, No.2 超高效液相色谱-串联质谱法快速检测水产品中喹 乙醇及其代谢物3-甲基-喹噁啉-2-羟酸的残留 1,2 2 2 2 2 1 薛良辰 ，彭玉芬 ，刘陆 ，蔡勤仁 ，冯家望 ，余以刚 （1.华南理工大学轻工与食品学院，广东广州 510640）（2.珠海出入境检验检疫局技术中心，广东珠海 519015） 摘要：建立了水产品中喹乙醇（OQX ）及其代谢物3-甲基-喹噁啉-2-羟酸（MQCA）的超高效液相色谱串联质谱快速测定方法。 试样经乙酸乙酯+ 乙腈（1+1，V/ V）液液萃取提取和净化后，BEH C18 UPLC进行分离，多反应选择离子检测。方法的回收率和变异系 数分别在62.5%~91.4%和2.6%~11.8%之间。本方法对水产品中喹乙醇和3- 甲基喹噁啉-2-羧酸的检测限均为1.0 μg/kg。 关键词：超高效液相色谱串联质谱；喹乙醇；3- 甲基-喹噁啉-2-羟酸；残留 文章篇号：1673-9078(2013)2-413-415 Rapid Determination of the Residues of Olaquindox and 3-methylquinoline-2-carboxylic Acid in Aquatic Products by UPLC-MS/MS 1,2 2 2 2 2 1 XUE Liang-chen , PENGYu-fen , LIU Lu ,CAI Qin-ren , FENG Jia-wang , YU Yi-gang (1.College of Light Industry and Food Sciences , South China University of Technology, Guangzhou 510640, China) (2.Zhuhai Inspection Quarantine Bureau, Zhuhai 519015, China) Abstract: This study presented a ultra performance liquid chromatography tandem mass spectrometry (UPLC -MS/MS) method for fast determination of the residues of olaquindox and 3-methylquinoline-2-carboxylic acid in aquatic products. Resident of olaquindox and 3-methylquinoline-2-carboxylic acid ware extracted by the liquid- liquid method using ethyl acetate+ acetonitrile （1+1, V/ V）.After BEH C18 LC gradient elution separation,the analytes ware determined under multi-reaction monitoring (MRM) scan type with tandemmass analyzer using positive polarity mode. The recoveries are in the range of 62.5%~91.4%, the relative standard deviation are in the range of 2.6%~11.8%. The limit of detection (LOD) fo