石墨烯-管尖固相萃取-高效液相色谱-串联质谱法测定贝类中3种原多甲藻酸贝类毒素  

Determination of Three Azaspiracids in Shellfish by Graphene-Based Pipette Tip Extraction Coupled with High Liquid Chromatography-Tandem Mass Spectrometry

作　　者：万译文[1,3] 杨霄 黄向荣[1,2,3] 索纹纹 何咏[1,3] 曾春芳 WAN Yiwen;YANG Xiao;HUANG Xiangrong;SUO Wenwen;HE Yong;ZENG Chunfang(Hunan Fisheries Science Institute,Changsha 410153;Collaborative Innovation Center for Efficient and Health Production of Fisheries in Hunan,Changde 415000;Fishery Products Quality Supervision and Testing Center,Ministry of Agriculture,Changsha 410153)

机构地区：[1]湖南省水产科学研究所,湖南长沙410153 [2]水产高效健康生产湖南省协同创新中心,湖南常德415000 [3]农业部渔业产品质量监督检验测试中心(长沙),湖南长沙410153

出　　处：《分析科学学报》2020年第3期324-330,共7页Journal of Analytical Science

摘　　要：本实验以石墨烯为吸附剂,制作了石墨烯-管尖固相萃取装置,结合高效液相色谱-串联质谱(HPLC-MS/MS)技术,建立了一种同时测定贝类中3种原多甲藻酸贝类毒素的分析方法。样品采用90%的甲醇提取,正己烷去脂,乙酸乙酯反萃取,石墨烯-管尖固相萃取净化,Kinetex XB-C18色谱柱(100 mm×2.1 mm,2.6μm)分离,在电喷雾正离子模式下,以选择反应监测方式测定,外标法定量。结果表明,贝类中3种原多甲藻酸毒素在1.0~100μg/kg的范围内线性良好,相关系数均大于0.99,定量限(LOQ)均为1.0μg/kg;在1.0μg/kg、5.0μg/kg和50μg/kg 3个加标水平的添加下,回收率在78.5%~102%之间,相对标准偏差小于15%。该方法具有灵敏、简单、快速等特点,适用于贝类水产品中3种原多甲藻酸毒素的分析检测。A method for the simultaneous determination of three azaspiracids(AZA1,AZA2 and AZA3)was developed based on graphene-based pipette tip solid-phase extraction(G-PT-SPE)coupled with high liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The samples were extracted with 90%methanol,defatted with n-hexane,backextracted with ethyl acetate and purified by G-PT-SPE.The extract was separated on a Kinetex XB-C18 column(100 mm×3.0 mm,1.8μm),and determined by tandem mass spectrometry operated in selected-reaction monitoring(SRM)mode with electrospray detector through positive ion scanning.Quantitative analysis method was external standard method.The calibration curves of three AZAs were linear in the range from 1.0μg/kg to 100μg/kg,with the correlation coefficients greater than 0.99,and the limits of quantifications(LOQs)were 1.0μg/kg,respectively.The average recoveries of three AZAs at the levels of 1.0μg/kg,5.0μg/kg,and 50μg/kg ranged from 78.5%to 102%,and the relative standard deviations were less than 15%.The method is sensitive,simple and rapid,and can be used for the determination of AZAs in shellfish products.

关 键 词：石墨烯 管尖固相萃取 高效液相色谱-串联质谱 原多甲藻酸贝类毒素 贝类 

分 类 号：O657.63[理学—分析化学]