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Method development for comprehensive extraction and analysis of marine toxins: Liquid-liquid extraction and tandem liquid chromatography separations coupled to electrospray tandem mass spectrometry
Talanta ( IF 5.6 ) Pub Date : 2018-05-09 , DOI: 10.1016/j.talanta.2018.05.019
David S. Wunschel , Blandina R. Valenzuela , Brooke L.Deatherage Kaiser , Kristin Victry , Dana Woodruff

A variety of toxins are produced by marine and freshwater microorganisms that present a threat to human health. These toxins have diverse chemical properties and specifically, a range of hydrophobicity. Methods for extraction and identification of these toxins are often geared toward specific classes of toxin depending on the sample type. There is a need for a general method of toxin extraction and identification for screening samples where the likely toxin content is not known a priori. We have applied a general method for metabolite extraction to toxin containing samples. This method was coupled with a simple dual liquid chromatography approach for separating a broad range of toxins. This liquid chromatography approach was coupled to triple quadrupole and quadrupole time-of-flight MS/MS platforms. The method was testing on a fish matrix for recovery of palytoxin as well as marine corals for detection of natural mixtures of palytoxin analogues. The recovery of palytoxin was found to produce a linear response (R2 of 0.95) when spiked into the fish matrix with a limit of quantitation of 2.5 ng/μL and recovery efficiency of 73% + /- 9%. The screening of corals revealed varying amount of palytoxin, and in one case, different palytoxin structural analogues. This demonstration illustrates the potential utility of this method for toxin extraction and detection.



中文翻译:

全面提取和分析海洋毒素的方法开发:液-液萃取和串联液相色谱分离与电喷雾串联质谱联用

海洋和淡水微生物会产生多种毒素,对人体健康构成威胁。这些毒素具有多种化学性质,尤其是一定范围的疏水性。这些毒素的提取和鉴定方法通常取决于样品类型,针对特定类别的毒素。需要一种通常的毒素提取和鉴定方法来筛选样品,其中先验未知的可能的毒素含量。我们已经应用了代谢物提取含毒素样品的通用方法。该方法与简单的双重液相色谱方法相结合,可分离多种毒素。这种液相色谱方法与三重四极杆和四极杆飞行时间MS / MS平台耦合。该方法是在鱼类基质上测试是否回收了palytoxin,以及在海洋珊瑚上进行了检测,以检测到palytoxin类似物的天然混合物。发现palytoxin的恢复产生线性响应(R 2浓度为2.5 ng /μL,回收效率为73%±9%时,加入鱼基质中时为0.95)。珊瑚的筛选显示了不同数量的palytoxin,在一种情况下,还显示了不同的palytoxin结构类似物。该演示说明了该方法在毒素提取和检测中的潜在效用。

更新日期:2018-05-09
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