SPE-UPLC-MS/MS联用测定水产品四环素类残留量  

Determination of Tetracycline Residues in Aquatic Products by SPE-UPLC-MS/MS

作　　者：叶瑞洪 黄迪惠[1,2] 刘珊珊 YE Ruihong;HUANG Dihui;LIU Shanshan(Fuqing Branch of Fujian Normal University,Fuqing,Fujian,350300,China)

机构地区：[1]福建师范大学福清分校海洋与生化工程学院,福建福清350300 [2]福建师范大学福清分校近海流域环境测控治理福建省高校重点实验室,福建福清350300

出　　处：《福建师大福清分校学报》2018年第5期56-62,91,共8页Journal of Fuqing Branch of Fujian Normal University

基　　金：福建省自然科学基金(2016J05030)

摘　　要：建立固相萃取净化-超高效液相色谱-串联质谱法测定水产品中四环素族中四环素、土霉素、金霉素和强力霉素四种抗生素残留量的检测方法 .采用固相萃取法(SPE),使样品经过Waters Oasis HLB固相萃取柱子吸附富集、净化和洗脱.在液相色谱-串联质谱(HPLC-MS/MS)多反应监测(MRM)正负离子切换模式测定水产品中四环素残留.结果表明四环素类在浓度10～200μg/L浓度范围里呈现良好的线性关系(相关系数r为0.9986～0.9993);检出限为2ng/mL;回收率为75.46%～103.86%;相对标准偏差(RSD)为0.40%～4.66%;此方法简便快捷,准确且稳定,适用于水产品中四环素类残留的测定.The tetracycline, oxytetracycline, chlortetracycline and doxycycline residues in aquatic products were measured by the combination of SPE and UPLC-MS/MS. The solid phase extraction（SPE） method was used to absorb, purify and elute the sample through Waters Oasis HLB. Determination of tetracycline residues in aquatic products was established according to the switching modes of positive and negative ion by the liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） and multiple reaction monitoring （MRM）. The results indicate that the tetracycline shows a good linear relationship in the concentration range from 10μg/L to 200μg/L, with the related coefficient ranging from 0.9986 to 0.9993, the detection limit 2ng/mL, and the recovery rate from 75.46% to 103.86%, and the relative standard deviation （RSD） from 0.40% to 4.66%. This method is simple, rapid, accurate, and stable, which is suitable for the determination of tetracycline residues in aquatic products.

关 键 词：四环素类 水产品 高效液相色谱-串联质谱 残留 

分 类 号：O656.31[理学—分析化学]