Palytoxin in seafood by liquid chromatography tandem mass spectrometry: investigation of extraction efficiency and matrix effect
Palytoxin in seafood by liquid chromatography tandem mass spectrometry: investigation of extraction efficiency and matrix effect
复制标题
DOI：
10.1007/s00216-011-5135-8
复制
发表时间：
2011-08-01
影响因子：
4.3
通讯作者：
Serpe, Luigi
中科院分区：
文献类型：
--
作者：
Ciminiello, Patrizia;Dell'Aversano, Carmela;Serpe, Luigi
据报道，在西班牙、法国、意大利和希腊的地中海沿岸出现了Ostreopsis属植物的大量繁殖，对人类健康构成严重威胁。Ostreopsis spp.的出现可能会导致海产品中的孢毒素污染，为了防止卫生风险，需要开发有效的提取程序，并结合海产品中孢毒素样化合物的快速敏感监测方法。研究了从海产品中提取palytoxin的最佳工艺条件和液相色谱串联质谱法（LC-MS/MS）对palytoxin进行定量分析的最佳工艺条件。选择三种海产品基质（贻贝、海胆和凤尾鱼），测试五种不同的提取体系，即：亲脂毒素提取的官方方案和各种甲醇或乙腈水溶液（MeOH/H2O 1:1、MeOH/H2O 8:2、men /H2O 8:2和MeOH 100%）。在LC-MS/MS检测palytoxin时，以MeOH/H2O 8:2为萃取液的提取精度和基质干扰最佳。对所有选定基质的准确性和日内重现性（n = 3）进行了评估，但仅对三种峰值浓度水平的贻贝进行了评估，其中包括共同体参考实验室提出的海洋生物毒素临时限量（250 μ g kg(-1)）。采用基质匹配标准计算贻贝、海胆和凤尾鱼组织中孢毒素的定量限；以MeOH/H2O 8:2的萃取效率计算，分别为228、343和500 μ g kg（-1）。
Blooms of Ostreopsis spp. have been recently reported along the Mediterranean coasts of Spain, France, Italy, and Greece posing serious risks to human health. Occurrence of Ostreopsis spp. may result in palytoxin contamination of seafood and, in order to prevent sanitary risks, the need exists to develop efficient extraction procedures to be coupled to rapid and sensitive monitoring methods of palytoxin-like compounds in seafood. In the present study, the best conditions for both extraction of palytoxin from seafood and palytoxin quantification by using liquid chromatography tandem mass spectrometry (LC-MS/MS) were investigated. Three seafood matrices (mussels, sea-urchins, and anchovies) were selected and five different extraction systems were tested, namely: the official protocol for extraction of lipophilic toxins and various aqueous methanol or acetonitrile solutions (MeOH/H2O 1:1, MeOH/H2O 8:2, MeCN/H2O 8:2 and MeOH 100%). Extraction with MeOH/H2O 8:2 provided the best results in terms of accuracy and matrix interference on LC-MS/MS detection of palytoxin. Accuracy and intra-day reproducibility (n = 3) were evaluated for all the selected matrices but only for mussels at three spiking concentration levels, including the provisional limit proposed by the Community Reference Laboratory for marine biotoxins (250 mu g kg(-1)). Limits of quantitation of palytoxin in mussels, sea-urchins and anchovies tissues were calculated using matrix-matched standards; taking into account extraction efficiency of MeOH/H2O 8:2, they resulted to be 228, 343, and 500 mu g kg(-1), respectively.