LC-MS/MS Analysis of the Emerging Toxin Pinnatoxin-G and High Levels of Esterified OA Group Toxins in Galician Commercial Mussels
LC-MS/MS Analysis of the Emerging Toxin Pinnatoxin-G and High Levels of Esterified OA Group Toxins in Galician Commercial Mussels
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DOI：
10.3390/toxins11070394
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发表时间：
2019-07-01
期刊：
影响因子：
4.2
通讯作者：
Botana, Luis M.
中科院分区：
文献类型：
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作者：
Otero, Paz;Miguens, Natalia;Botana, Luis M.
海洋有害藻类的出现在世界范围内不断增加，因此，有害浮游植物中亲脂性海洋毒素的积累对贝类行业的食品安全构成威胁。加利西亚是欧盟重要的食用双壳软体动物生产国，在过去的几十年里，贻贝养殖场关闭的情况屡屡发生。这项工作旨在研究商业贻贝（Mytilus galloprovincialis）的毒性特征，以确定摄入时的潜在风险。为此，通过液相色谱串联质谱 (LC-MS/MS) 对 3 个里亚斯（阿瑞斯萨达、阿鲁萨和庞特维德拉）养殖并在 5 个当地市场购买的总共 41 个贻贝样本进行了分析。色谱图显示存在大田酸 (OA)、恐龙毒素-2 (DTX-2)、果胶毒素-2 (PTX-2)、氮杂螺酸-2 (AZA-2) 和新出现的毒素 13-去甲基螺内酯 C (SPX-13) 和羽衣藻毒素-G (PnTX-G)。每种毒素的定量是使用其自己的标准校准在 0.1%-50 ng/mL (R2 > 0.99) 范围内确定的，并考虑毒素回收率 (62-110%) 和基质校正 (33-211%)。数据显示，OA和DTX-2（尤其是酯类）是加利西亚软体动物的主要风险，在38个样品（93%）中检出，其中3个样品超出法定限量（160微克/公斤），其次是SPX-13，在19个样品（46%）中检出，含量高达28.9微克/公斤。 PTX-2、AZA-2 和 PnTX-G 的分析表明含量较小。 15 个样品（37%）PTX-2（0.7-2.9 μg/kg）阳性，12 个样品（29%）AZA-2（0.1-1.8 μg/kg）阳性，5 个贻贝样品（12%）检测到 PnTX-G（0.4 μg/kg-0.9 μg/kg）。这是加利西亚软体动物首次被 PnTX-G 污染。尽管结果表明这种毒素不是贻贝摄入的潜在风险，但应在通过 LC-MS/MS 方法进行的贝类安全监测计划中考虑它。
The occurrence of marine harmful algae is increasing worldwide and, therefore, the accumulation of lipophilic marine toxins from harmful phytoplankton represents a food safety threat in the shellfish industry. Galicia, which is a commercially importantEUproducer of edible bivalvemollusk have been subjected to recurring cases of mussel farm closures, in the last decades. This work aimed to study the toxic profile of commercial mussels (Mytilus galloprovincialis) in order to establish a potential risk when ingested. For this, a total of 41 samples of mussels farmed in 3 Rias (Ares-Sada, Arousa, and Pontevedra) and purchased in 5 localmarketswere analyzed by liquid chromatography tandemmass spectrometry (LC-MS/MS). Chromatograms showedthepresence of okadaic acid(OA), dinophysistoxin-2 (DTX-2), pectenotoxin-2 (PTX-2), azaspiracid-2 (AZA-2), and the emerging toxins 13-desmethyl spirolide C (SPX-13), and pinnatoxin-G (PnTX-G). Quantification of each toxin was determined using their own standard calibration in the range 0.1%-50 ng/mL (R2 > 0.99) and by considering the toxin recovery (62-110%) and the matrix correction (33-211%). Data showed that OA and DTX-2 (especially in the form of esters) are the main risk in Galician mollusks, which was detected in 38 samples (93%) and 3 of them exceeded the legal limit (160 mu g/kg), followed by SPX-13 that was detected in 19 samples (46%) in quantities of up to 28.9 mu g/kg. Analysis from PTX-2, AZA-2, and PnTX-G showed smaller amounts. Fifteen samples (37%) were positive for PTX-2 (0.7-2.9 mu g/kg), 12 samples (29%) forAZA-2 (0.1-1.8 mu g/kg), and PnTX-G was detected in 5 mussel samples (12%) (0.4 mu g/kg-0.9 mu g/kg). This is the first time Galician mollusk was contaminated with PnTX-G. Despite results indicating that this toxin was not a potential risk through the mussel ingestion, it should be considered in the shellfish safety monitoring programs through the LC-MS/MS methods.