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Open AccessArticle

Combined (d)SPE-QuEChERS Extraction of Mycotoxins in Mixed Feed Rations and Analysis by High Performance Liquid Chromatography-High-Resolution Mass Spectrometry

1
Galician Agency for Food Quality—Agronomic and Agrarian Research Centre (AGACAL-CIAM), Unit of Organic Contaminants, Apartado 10, 15080 A Coruña, Spain
2
Laboratory of Research and Development of Analytical Solutions (LIDSA), Department of Analytical Chemistry, Nutrition and Food Science, Faculty of Chemistry, E-15782 Campus Vida, Universidad de Santiago de Compostela, 15782 Santiago de Compostela, Spain
*
Author to whom correspondence should be addressed.
Toxins 2020, 12(3), 206; https://doi.org/10.3390/toxins12030206 (registering DOI)
Received: 16 December 2019 / Revised: 12 March 2020 / Accepted: 13 March 2020 / Published: 23 March 2020
(This article belongs to the Special Issue Application of LC-MS/MS in the Mycotoxins Studies)
The objective of this work was the development of a methodology capable of simultaneously determine 26 mycotoxins in mixed feed rations collected in 20 dairy farms. A sample preparation methodology based on a combination of (d)SPE and QuEChERS extractions was used. Liquid chromatography-high resolution mass spectrometry was employed for both identification and quantification purposes. To this respect, a powerful workflow based on data-independent acquisition, consisting of fragmenting all precursor ions entering the mass spectrometer in narrow m/z isolation windows (SWATH), was implemented. SWATH data file then contains all the information that would be acquired in a multitude of different experimental approaches in a single all-encompassing dataset. Analytical method performance was evaluated in terms of linearity, repeatability and matrix effect. Relative recoveries were also measured, giving values above 80% for most compounds. Matrix-matched calibration was carried out and enabled reaching the low ng mL−1 level for many mycotoxins. The observed matrix effect, in most cases suppressive, reached even values higher than 60%. The repeatability was also adequate, showing a relative standard deviation lower than 10%. All unified samples analyzed showed co-occurrence of two or more mycotoxins, recurrently zearalenone, fumonisin B1, and β-zearalenol, with an occurrence frequency ranging from 60% to 90%. View Full-Text
Keywords: Mycotoxins; mixed feed rations; QuEChERS; dispersive solid phase extraction; liquid chromatography; high-resolution mass spectrometry; data independent SWATH Mycotoxins; mixed feed rations; QuEChERS; dispersive solid phase extraction; liquid chromatography; high-resolution mass spectrometry; data independent SWATH
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MDPI and ACS Style

Facorro, R.; Llompart, M.; Dagnac, T. Combined (d)SPE-QuEChERS Extraction of Mycotoxins in Mixed Feed Rations and Analysis by High Performance Liquid Chromatography-High-Resolution Mass Spectrometry. Toxins 2020, 12, 206.

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