期刊
TOXINS
卷 12, 期 3, 页码 -出版社
MDPI
DOI: 10.3390/toxins12030206
关键词
Mycotoxins; mixed feed rations; QuEChERS; dispersive solid phase extraction; liquid chromatography; high-resolution mass spectrometry; data independent SWATH
资金
- CONECTA-PEME GALAC project [IN852A 2016/103]
- Infrastructure Program, MINECO, Spain [IGDC13-1E-2026]
- Galician Competitive Research Groups [GPC 2017/04, GPC IN607B 2019/13]
- CRETUS Strategic Partnership [ED431E 2018/01]
- FEDER (UE)
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 beta-zearalenol, with an occurrence frequency ranging from 60% to 90%.
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