Villar-González A, Rodríguez-Velasco M L, Ben-Gigirey B, Botana L M
EU-Community Reference Laboratory for Marine Biotoxins, Agencia Española Seguridad Alimentaria y Nutrición (AESAN), Estación Marítima s/n, 36200 Vigo, Spain.
Toxicon. 2007 Jun 15;49(8):1129-34. doi: 10.1016/j.toxicon.2007.02.002. Epub 2007 Feb 16.
By the end of 2005, a toxic episode of phytoplankton origin in bivalve shellfish led to the closing down of several shellfish production areas in Galicia (northwestern region of Spain). During this time, different kinds of shellfish were collected and analysed by LC-MS/MS to search for the following lipophilic toxins: okadaic acid (OA), dinophysistoxins (DTXs), pectenotoxins (PTXs), azaspiracids (AZAs) and spirolides. Samples were analysed before alkaline hydrolysis in order to investigate the presence of free OA and DTXs, AZAs, PTXs and spirolides, and after alkaline hydrolysis to detect OA and DTXs esters. All of the samples were found to be contaminated with OA and/or DTX-2, as well as esterified forms of these diarrhetic shellfish poison (DSP) toxins, at levels around and above European regulatory limit (160 microg of okadaic acid equivalents/kg). The analyses of mussels and razor clam also revealed the presence of 13-desmethyl spirolide C (SPX-1) at levels below 31 microg/kg. Likewise, in many of the samples different levels of pectenotoxin-2 secoacid (PTX-2sa) were detected. DSP toxin esters represent practically the 100% of the total OA equivalents for scallops, clams, razor clams and cockles.
到2005年底，一起源自浮游植物的毒性事件导致加利西亚（西班牙西北部地区）的几个贝类产区关闭。在此期间，采集了不同种类的贝类，并用液相色谱-串联质谱法进行分析，以寻找以下亲脂性毒素：冈田酸（OA）、鳍藻毒素（DTXs）、pectenotoxins（PTXs）、azaspiracids（AZAs）和spirolides。在碱性水解之前对样品进行分析，以调查游离OA、DTXs、AZAs、PTXs和spirolides的存在情况，碱性水解之后进行检测以发现OA和DTXs酯。所有样品均被发现受到OA和/或DTX-2以及这些腹泻性贝类毒素（DSP）的酯化形式的污染，污染水平达到或超过欧洲监管限值（160微克冈田酸当量/千克）。贻贝和蛏子的分析还显示存在水平低于31微克/千克的13-去甲基spirolide C（SPX-1）。同样，在许多样品中检测到了不同水平的pectenotoxin-2 secoacid（PTX-2sa）。对于扇贝、蛤蜊、蛏子和鸟蛤，DSP毒素酯实际上占总OA当量的100%。
