水产品中11种海洋生物毒素的高效液相色谱-四极杆/静电场轨道阱高分辨质谱检测方法研究  

Study on Detection of Eleven Marine Biotoxins in Seafood by High Performance Liquid Chromatography-Quadrupole Electrostatic Field Orbitrap High-resolution Mass Spectrometry

作　　者：方科益 陈树兵 李双 徐旭文 周虹玲 李露青 曹国洲 陈先锋 FANG Ke-yi;CHEN Shu-bing;LI Shuang;XU Xu-wen;ZHOU Hong-ling;LI Lu-qing;CAO Guo-zhou;CHEN Xian-feng(Technology Center of Ningbo Customs,Ningbo 315040,China;Ningbo Zhongsheng Product Testing Company,Ningbo 315040,China)

机构地区：[1]宁波海关技术中心,浙江宁波315040 [2]宁波中盛产品检测公司,浙江宁波315040

出　　处：《分析测试学报》2019年第9期1091-1096,共6页Journal of Instrumental Analysis

基　　金：原国家质检总局科技计划项目(2017IK070);浙江省基础公益研究计划项目(LGN18B050002);宁波市科技创新团队(2015C110018)

摘　　要：建立了水产品中11种海洋生物毒素的高效液相色谱-四极杆/静电场轨道阱高分辨质谱(HPLC-Q-Orbitrap HRMS)检测方法。该方法采用分级提取原理,结合分散固相萃取技术(dSPE)和载体辅助液液萃取技术(SLLE),建立了对亲水性及亲脂性海洋生物毒素的“一站式”提取净化体系。在优化条件下,11种毒素在一定质量浓度范围内具有良好的线性关系,相关系数(r)均大于0.99。该方法对11种毒素的检出限为1~10μg/kg,定量下限为2~20μg/kg,加标回收率为55.6%~122%,相对标准偏差为5.4%~16%。方法快速高效,可操作性强,解决了不同理化性质的海洋生物毒素的通用性检测问题,可满足水产品中海洋生物毒素的快速筛查要求。A method was established for the determination of 11 marine biotoxins in seafood by high-performance liquid chromatography-quadrupole electrostatic field-orbitrap high-resolution mass spectrometry(HPLC-Q-Orbitrap HRMS).It was a one-stop extraction and purification system for hydrophilic and lipophilic marine biotoxins.Samples were firstly treated by sequential extraction procedure,then cleaned up by disperse solid phase extraction(dSPE)combined with carrier-assisted liquid-liquid extraction(SLLE).Under the optimal conditions,the calibration curves for 11 marine biotoxins were linear in the certain concentration ranges,with correlation coefficients greater than 0.99.The limits of detection(LOD)and limits of quantitation(LOQ)were in the ranges of 1-10μg/kg and 2-20μg/kg,respectively.The spiked recoveries ranged from 55.6%to 122%with relative standard deviations(RSD)of 5.4%-16%.The method was simple,efficient and operable,and could solve the problem of high-throughput detection of hydrophilic and lipophilic marine biotoxins in seafood and meet the requirements for rapid screening.

关 键 词：海洋生物毒素 分散固相萃取(dSPE) 载体辅助液液萃取(SLLE) 高效液相色谱-四极杆/静电场轨道阱高分辨质谱(HPLC-Q-Orbitrap HRMS) 

分 类 号：O657.63[理学—分析化学] S852.44[理学—化学]