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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
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作者单位
方科益,陈树兵,李双,徐旭文,周虹玲,李露青,曹国洲,陈先锋 1.宁波海关技术中心2.宁波中盛产品检测公司 
基金项目: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)
中文摘要: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1~10 μg/kg,定量下限为2~20 μg/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。
中文关键词: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)
 
Study on Detection of Eleven Marine Biotoxins in Seafood by High Performance Liquid Chromatography-Quadrupole Electrostatic Field Orbitrap High resolution Mass Spectrometry
Abstract: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 1-10 μg/kg and 2-20 μg/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.
Key Words:marine biotoxins  dispersed solid phase extraction(dSPE)  carrier assisted liquid-liquid extraction(SLLE)  high-performance liquid chromatography-quadrupole electrostatic field orbitrap high resolution mass spectrometry(HPLC-Q-Orbitrap HRMS)
引用本文:方科益,陈树兵,李双,徐旭文,周虹玲,李露青,曹国洲,陈先锋.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[J].分析测试学报,2019,(9):1091-1096.
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