ASE/UPLC-MS/MS测定海产品中17种海洋脂溶性藻毒素  

Determination of 17 Marine Lipophilic Phycotoxins in Seafood Using Accelerated Solvent Extraction Combined with Ultrahigh Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：李静 麦艳玲 肖陈贵 沈金灿 李文涛 郭建宁 钟润生[1] 李杨 LI Jing;MAK Yim-ling;XIAO Chen-gui;SHEN Jin-can;LI Wen-tao;GUO Jian-ning;ZHONG Run-sheng;LI Yang(Department of Transportation and Environment,Shenzhen Institute of Information Technology,Shenzhen 518172,China;State Key Laboratory of Marine Pollution(SKLMP),City University of Hong Kong,Hong Kong 999077,China;Key Laboratory of Detection Technology R&D on Food Safety,Food Inspection and Quarantine Technology Center of Shenzhen Customs,Shenzhen 518026,China)

机构地区：[1]深圳信息职业技术学院交通与环境学院,广东深圳518172 [2]香港城市大学海洋污染国家重点实验室,中国香港999077 [3]深圳海关食品检验检疫技术中心深圳市食品安全检测技术研发重点实验室,广东深圳518026

出　　处：《分析测试学报》2024年第12期1952-1958,共7页Journal of Instrumental Analysis

基　　金：深圳科技创新稳定支持计划(KJ2024C006)。

摘　　要：建立了快速溶剂萃取/超高效液相色谱-串联质谱(ASE/UPLC-MS/MS)同时检测17种海洋脂溶性藻毒素(MLPs)的方法。鱼贝类海产品采用甲醇在高温高压下进行快速萃取,再依次采用反相Agilent Bond Elut C_(18)(500 mg/6 mL)和Waters Sep-Pak(500 mg/6 mL)正相硅胶固相萃取小柱进行净化;以含有0.1%甲酸和2 mmol/L甲酸铵的95%乙腈和水为流动相,使用Phenomenex Kinetex C_(18)色谱柱(100 mm×2.1 mm,1.7μm)进行分离,在电喷雾电离多反应监测模式下同时检测,17种MLPs在6 min内全部被洗脱并检测。17种MLPs的相关系数为0.994 9~0.999 9,定量下限为0.020~30 pg/g湿重(ww)。在6种海产品中,17种MLPs的加标回收率为67.3%~116%,相对标准偏差(RSD)不大于15%。采用该方法对采自我国南海的11个鱼类、21个甲壳动物、19个软体动物样品进行测定,共检出12种MLPs,总含量为316~20 300 pg/g ww,主要为大田软骨酸毒素(OA)、鳍藻毒素(DTXs)和虾夷扇贝毒素(YTXs)。该方法具有优良的准确度和精密度,满足实际海产品中17种MLPs的同时检测要求。A method was established for the simultaneous detection of 17 marine lipophilic phycotoxins(MLPs) by ultrahigh performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) combined with accelerated solvent extraction(ASE),including azaspiracids(AZAs),brevetoxins(BTXs),ciguatoxins(CTXs),dinophysistoxins(DTXs),gymnodimine(GYM),okadaic acid(OA),spirolides(SPXs),pectenotoxins(PTXs) and yessotoxins(YTXs).Seafood was extracted by accelerated solvent extraction with methanol,and then purified by reverse phase(Agilent Bond Elut C_(18),500 mg/6 mL) and normal phase solid phase(Waters Sep-Pak,500 mg/6 mL) extraction cartridges subsequently.Mobile phase was water and 95% acetonitrile(95∶5,volume ratio),both of which contained 0.1% formic acid and 2 mmol/L ammonium formate.A Phenomenex Kinetex C_(18) LC column(100 mm×2.1 mm,1.7 μm) was performed to separate the lipophilic phycotoxins in six minutes and then the target analytes were detected by UPLC-MS/MS in multiple reaction monitoring mode.The correlation coefficients of standard curves were 0.994 9-0.999 9 and the method quantification limits of 17 MLPs ranged from 0.020 to 30 pg/g ww.The matrix-spiked recoveries of 17 MLPs ranged from 67.3% to 116% with the relative standard deviations below 15%.Twelve lipophilic phycotoxins were detected in seafood from South China Sea,with the total concentration ranging from 316to 20 300 pg/g ww.This method presents good sensitivity and precision,which can satisfy the requirements for simultaneous determination of 17 MLPs in seafood.

关 键 词：超高效液相色谱-串联质谱 快速溶剂萃取 固相萃取 海洋脂溶性藻毒素 海产品 

分 类 号：O657.7[理学—分析化学] TS207.3[理学—化学]