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Identification and quantification of domoic acid by UHPLC/ QTOF tandem mass spectrometry, with simultaneous identification of non-target photodegradation products

机译:通过UHPLC / QTOF串联质谱法鉴定和定量海藻酸,同时鉴定非目标光降解产物

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摘要

Amnesic shellfish poisoning is a potentially lethal human toxic syndrome which is caused by domoic acid (DA), a neurotoxin produced by marine phytoplankton, principally from Pseudonitzschia genus. In this report, a method to identify and quantify the DA toxin, with simultaneous identification of its photodegradation products, has been developed. It uses an ultra high performance liquid chromatography coupled to a quadrupole-time-of-flight tandem mass spectrometer (UHPLC-QTOF) after solid-phase extraction (SPE). An unambiguous identification of DA was carried out by considering both the retention time of DA in UHPLC and the exact mass of protonated DA molecule ([M+H](+)=312.1447m/z) and of the most intense fragment ion (m/z 266.1391). The quantification was conducted using protonated DA molecule with protonated Glafenin as internal standard, obtaining a limits of detection of 0.75 mu g L-1. Large screening with UHPLC-QTOF could also give structural information about degradation products of DA present in samples after UV-irradiation. This method was applied for the determination of DA in complex liquid samples after SPE and is applicable for environmental monitoring of this toxic substance in the aquatic environment.
机译:失忆性贝类中毒是一种潜在的致命人类毒性综合症,由多摩酸(DA)引起,多摩酸是海洋浮游植物产生的一种神经毒素,主要来自假单胞菌属。在本报告中,已经开发了一种鉴定和定量DA毒素,同时鉴定其光降解产物的方法。在固相萃取(SPE)后,它使用超高效液相色谱与四极杆飞行时间串联质谱仪(UHPLC-QTOF)结合使用。考虑到DA在UHPLC中的保留时间以及质子化DA分子的精确质量([M + H](+)= 312.1447m / z)和最强碎片离子(m / z 266.1391)。使用质子化DA分子和质子化的Glafenin作为内标进行定量,检测限为0.75μg L-1。使用UHPLC-QTOF进行的大规模筛选还可以提供有关UV照射后样品中存在的DA降解产物的结构信息。该方法用于固相萃取后复杂液体样品中DA的测定,可用于水生环境中该有毒物质的环境监测。

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