title: Development and validation of an UHPLC-MS/MS method for the determination of mycotoxins in grass silages.
abstract: An ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) multi-mycotoxin analytical method was developed to simultaneously identify and quantify 20 mycotoxins in grass silages, inclusive of mycotoxins that are currently regulated in European Union feeds. Extraction of mycotoxins from dried grass silages was performed using of a modified QuEChERS extraction employing an acidified aqueous extraction (0.1 N HCl) with no further clean-up. Following chromatographic separation, analytes were detected using a fast polarity-switching MS/MS method that allowed both positive and negative ions to be analysed from a single injection, thus the reducing time and cost of analysis. The limits of detection and quantification ranged between 3 µg kg(-1) DM (aflatoxin B1, beauvericin and enniatin A and A1) and 200 µg kg(-1) DM (deoxynivalenol), and between 10 µg kg(-1) DM (aflatoxin B1, beauvericin and enniatin A1) and 500 µg kg(-1) DM (deoxynivalenol), respectively. Inter-assay accuracy and precision ranged between 90% and 107% and between 3.9% and 15.0% CV, respectively. The accuracy of the method was assessed through the application to a range of incurred samples in an inter-laboratory study.
authors.affiliation: a Animal & Grassland Research and Innovation Centre, Teagasc, Grange, Dunsany, Co. Meath , Ireland.|b Institute for Global Food Security , Queen's University Belfast , Belfast , Northern Ireland.|c Food Safety Department , Teagasc Food Research Centre , Ashtown , Dublin 15 , Ireland.
authors.forename: Cormac
authors.initials: C
authors.lastname: McElhinney
authors.affiliation: a Animal & Grassland Research and Innovation Centre, Teagasc, Grange, Dunsany, Co. Meath , Ireland.
authors.forename: Pádraig
authors.initials: P
authors.lastname: O'Kiely
authors.affiliation: b Institute for Global Food Security , Queen's University Belfast , Belfast , Northern Ireland.
authors.forename: Chris
authors.initials: C
authors.lastname: Elliott
authors.affiliation: c Food Safety Department , Teagasc Food Research Centre , Ashtown , Dublin 15 , Ireland.
authors.forename: Martin
authors.initials: M
authors.lastname: Danaher
mesh_terms: D016604:Aflatoxin B1 / Q000096:biosynthesis / Q000302:isolation & purification*; D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods / Q000592:standards; D047630:Depsipeptides / Q000096:biosynthesis / Q000302:isolation & purification*; D005506:Food Contamination / Q000032:analysis; D005658:Fungi / Q000472:pathogenicity / Q000502:physiology; D006851:Hydrochloric Acid / Q000737:chemistry; D057230:Limit of Detection; D059627:Liquid Phase Microextraction; D009183:Mycotoxins / Q000096:biosynthesis / Q000302:isolation & purification*; D010935:Plant Diseases / Q000382:microbiology; D006109:Poaceae / Q000737:chemistry* / Q000378:metabolism / Q000382:microbiology; D015203:Reproducibility of Results; D012820:Silage / Q000032:analysis; D053719:Tandem Mass Spectrometry / Q000379:methods / Q000592:standards; D014255:Trichothecenes / Q000096:biosynthesis / Q000302:isolation & purification*
chemical_list: D047630:Depsipeptides; D009183:Mycotoxins; D014255:Trichothecenes; C100264:enniatins; C004456:beauvericin; D016604:Aflatoxin B1; C007262:deoxynivalenol; D006851:Hydrochloric Acid
keywords: UHPLC-MS/MS; extraction; grass; mycotoxins; silage