ASE/UPLC-MS/MS 测定海产品中 17 种海洋脂溶性藻毒素

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 C₁₈, 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 C₁₈ LC column (100 mm×2. 1 mm, 1. 7 μµm) 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 316 to 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. © 2024, China Association for Instrumental Analysis. All rights reserved.