Quantification and profiling of lipophilic marine toxins in microalgae by UHPLC coupled to high-resolution orbitrap mass spectrometry

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• 作者：Gabriel Orellana ; Lieven Van Meulebroek…
• 关键词：Ultra ; high ; performance liquid chromatography high ; resolution Orbitrap mass spectrometry ; Plackett ; Burman ; Validation ; Harmful algae ; Yessotoxins ; Spirolide
• 刊名：Analytical and Bioanalytical Chemistry
• 出版年：2015
• 出版时间：August 2015
• 年：2015
• 卷：407
• 期：21
• 页码：6345-6356
• 全文大小：1,166 KB
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• 作者单位：Gabriel Orellana (1) (2)
  Lieven Van Meulebroek (1)
  Sarah Van Vooren (1)
  Maarten De Rijcke (2)
  Michiel Vandegehuchte (2)
  Colin R. Janssen (2)
  Prof. Dr. Ir. Lynn Vanhaecke (1)
  
  1. Faculty of Veterinary Medicine, Department of Veterinary Public Health and Food Safety, Laboratory of Chemical Analysis, Ghent University, Salisburylaan 133, 9820, Merelbeke, Belgium
  2. Laboratory of Environmental Toxicology and Aquatic Ecology, Ghent University, Jozef Plateaustraat 22, 9000, Ghent, Belgium
  
• 刊物类别：Chemistry and Materials Science
• 刊物主题：Chemistry
  Analytical Chemistry
  Food Science
  Inorganic Chemistry
  Physical Chemistry
  Monitoring, Environmental Analysis and Environmental Ecotoxicology
  
• 出版者：Springer Berlin / Heidelberg
• ISSN：1618-2650

文摘

During the last decade, a significant increase in the occurrence of harmful algal blooms (HABs), linked to repetitive cases of shellfish contamination has become a public health concern and therefore, accurate methods to detect marine toxins in different matrices are required. In this study, we developed a method for profiling lipophilic marine microalgal toxins based on ultra-high-performance liquid chromatography coupled to high-resolution Orbitrap mass spectrometry (UHPLC-HR-Orbitrap MS). Extraction of selected toxins (okadaic acid (OA), dinophysistoxin-1 (DTX-1), pectenotoxin-2 (PTX-2), azaspiracid-1 (AZA-1), yessotoxin (YTX) and 13-desmethyl spirolide C (SPX-1)) was optimized using a Plackett-Burman design. Three key algal species, i.e., Prorocentrum lima, Protoceratium reticulatum and Alexandrium ostenfeldii were used to test the extraction efficiency of OA, YTXs and SPXs, respectively. Prorocentrum micans, fortified with certified reference solutions, was used for recovery studies. The quantitative and confirmatory performance of the method was evaluated according to CD 2002/657/EC. Limits of detection and quantification ranged between 0.006 and 0.050?ng?mL? and 0.018 to 0.227?ng?mL?, respectively. The intra-laboratory reproducibility ranged from 6.8 to 11.7?%, repeatability from 6.41 to 11.5?% and mean corrected recoveries from 81.9 to 119.6?%. In addition, algae cultures were retrospectively screened for analogues and metabolites through a homemade database. Using the ToxID software programme, 18 toxin derivates were detected in the extract of three toxin producing microalgae species. In conclusion, the generic extraction and full-scan HRMS approach offers an excellent quantitative performance and simultaneously allows to profile analogues and metabolites of marine toxins in microalgae.