title: Analysis of mycotoxins in barley using ultra high liquid chromatography high resolution mass spectrometry: comparison of efficiency and efficacy of different extraction procedures.
abstract: The effectiveness of four extraction methods (modified QuEChERS, matrix solid-phase dispersion (MSPD), solid-liquid extraction (SLE) and solid-phase extraction (SPE) clean-up) were evaluated for simultaneous determination of 32 mycotoxins produced by the genus Fusarium, Claviceps, Aspergillus, Penicillium and Alternaria in barley by ultra high pressure liquid chromatography coupled to ultra-high resolution mass spectrometry (UHPLC-Orbitrap(®) MS). The efficiency and efficacy of extraction methods were evaluated and compared in number of extracted mycotoxins and obtained recoveries. From the one point of view, QuEChERS procedure was fast and easy, as well as it was able to successfully extract all selected mycotoxins. On the other hand, SLE method, MSPD and SPE clean-up method did not extract adequately all selected mycotoxins and recoveries were not suitable enough. Thereby, method employing QuEChERS extraction connected with UHPLC-Orbitrap(®) MS was developed to quantify 32 mycotoxins in barley within this study. Analytical method was validated and recoveries ranged from 72% to 101% for selected mycotoxins with only one exception nivalenol (NIV) and deoxynivalenol-3-glucoside (D3G), which were lower than 67%. Relative standard deviations (RSD) were lower than 17.4% for all target mycotoxins. The lowest calibration levels (LCLs) ranged from 1 to 100 μg/kg. Validated method was finally used for monitoring mycotoxins in a total of 15 Czech barley samples, when only Fusarium toxins representatives were detected in 53% of samples and the mycotoxins with the highest incidence were enniatins.
authors.affiliation: Departament de Medicina Preventiva, Facultat de Farmàcia, Universitat de Valencia, Av. Vicent Andrès Estellès s/n, 46100 Burjassot (València), Spain. josep.rubert@uv.es
authors.forename: Josep
authors.initials: J
authors.lastname: Rubert
authors.forename: Zbynek
authors.initials: Z
authors.lastname: Dzuman
authors.forename: Marta
authors.initials: M
authors.lastname: Vaclavikova
authors.forename: Milena
authors.initials: M
authors.lastname: Zachariasova
authors.forename: Carla
authors.initials: C
authors.lastname: Soler
authors.forename: Jana
authors.initials: J
authors.lastname: Hajslova
mesh_terms: D005591:Chemical Fractionation / Q000379:methods*; D002851:Chromatography, High Pressure Liquid; D005506:Food Contamination / Q000032:analysis*; D001467:Hordeum / Q000737:chemistry*; D013058:Mass Spectrometry; D009183:Mycotoxins / Q000032:analysis* / Q000302:isolation & purification*; D015203:Reproducibility of Results; D013997:Time Factors
chemical_list: D009183:Mycotoxins