Detection of 13 mycotoxins in feed using modified QuEChERS with dispersive magnetic materials and UHPLC–MS/MS

Abstract

An analytical method for the simultaneous determination of 13 mycotoxins in feed by magnetic dispersive solid-phase extraction combined with ultra-high performance liquid chromatography and tandem mass spectrometry was developed. The samples were extracted with acetonitrile/water (80:20, v/v, containing 3% acetic acid), and separated by centrifugation after salting-out, and then treated with magnetic adsorbents to remove interferences. The separation of target mycotoxins was performed on an ACQUITY UPLC HSS T3 column using a mobile phase consisting of 1 mmol/L ammonium acetate with 0.1% formic acid and methanol by gradient elution. Good linearities for the 13 mycotoxins were achieved with correlation coefficients over 0.99, and the recoveries of mycotoxins were in the range of 89.3-112.6% at spiking at levels of 5, 20, and 100 μg/kg, with relative standard deviations of 0.9-10.4%. Based on the functional magnetic materials (MDN@Fe O , PSA@Fe O , ZrO Fe O ) applied in dispersive solid-phase extraction, the pretreatment process is more convenient and it is beneficial to reduce the experimental cost by reusing the recycled magnetic materials. It is a simple, rapid, and environmentally friendly analytical method for the determination of mycotoxins in feed.

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

“…Most studies concerning mycotoxins occurrence were carried out in food matrices, cereals [5][6][7][8] feedstuff [1,9,10], plant based beverages [11], and ruminant milk [12]. Nonetheless, some researchers also found traces of these toxins in human breast milk [13,14].…”

“…From classic approaches like solid liquid extraction (SLE) and liquid-liquid extraction (LLE) to the most recent ones, like modified Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) extraction or matrix solid-phase dispersion (MSPD). Modified QuEChERS procedure is the sample pre-treatment of choice in many recent publications, due to its simplicity and cost-efficiency [8,9,19,20].…”

“…HPLC coupled to tandem mass spectrometry (MS/MS) is considered the most reliable technique in order to achieve high specificity and sensitivity for the simultaneous determination of a large number of mycotoxins, reaching low limits of detection (LOD) and quantification (LOQ). Several studies using this technique for the analysis of multi-mycotoxins in food and feed commodities have been published [9,10,12,26,27].…”

Multiple mycotoxins analysis in animal feed with LC‐MS/MS: Comparison of extract dilution and immunoaffinity clean‐up

“…The important factor is reliable, fit-for-purpose methods which allow surveillance of mycotoxin levels in different commodities [2]. Article Related Abbreviations: AFB 1 , aflatoxin B 1 ; AFLB1-IS, aflatoxin B1 13 C 17 ; DON, deoxynivalenol; FB 1 , fumonisin B 1 ; FB1-IS, fumonisin B1 13 C 34 ; FB 2 , fumonisin B 2 ; HT-2, HT-2 toxin; HT-2-IS, toxin HT-2 13 C 22 ; IAC, immunoaffinity chromatography; MIX8 VL, working standard solution for analytes; MIX8 VL IS, working standard solution for internal standards; OTA, ochratoxin A; PBS, phosphate buffered saline; T-2, T-2 toxins; T-2-IS, toxin T-2 13 For many years, liquid chromatography with fluorescence or UV detection were the "gold standard" in mycotoxin control. Most of the published and normalized methods were based on immunoaffinity clean-up [6,7] and allowed specific, singleanalyte analysis with sufficient performance.…”

“…Many authors have published multi-mycotoxin methods [9,[11][12][13][14][15][16] but only a few have used immunoaffinity columns developed for multi-analysis of food [17][18][19] and feed [20]. The main advantage of these columns is high clean-up potential, helpful in work with complex matrixes.…”