Abstract

High-performance thin-layer chromatography (HPTLC) and HPTLC coupled with mass spectrometry (MS) methods were described for the simultaneous determination of zearalenone (ZEA); type B trichothecenes (TCT-B); nivalenol (NIV) and deoxynivalenol (DON) along with its acetylated derivatives: 3-acetyldeoxynivalenol (3-ADON) and 15-acetyldeoxynivalenol (15-ADON). The extract samples were cleaned-up with Bond Elut Mycotoxin® solid-phase extraction cartridges. Then, separation was performed on HPTLC silica gel 60 F254 plates using toluene, ethyl acetate and formic acid (1:8:1 v/v/v) as mobile phase. Derivatisation was then performed with 10% aluminium trichloride in 50% methanol. Mycotoxin standards and spiked cereals grains were identified by UV spots at 366 nm, with retention factors (R F) of 0.20 (NIV), 0.39 (DON), 0.45 (15-ADON), 0.50 (3-ADON) and 0.60 (ZEA). Some parameters of validation were determined. Calibration data (n = 5) fitted a linear regression model with determination coefficients, R2 > 0.99. The recovery was determined in triplicate at two levels, ranging from 84.3 ± 2.2% to 114.2 ± 11.7%. Detection limits ranged from 80 to 120 μg kg−1 and quantification limits ranged from 120.0 to 200 μg kg−1. The analysis by HPTLC/electrospray (ESI)-MS in negative mode confirmed the presence of TCT-B and ZEA standards in Chilean cereals with mass signals at m/z 355, 371, 337, and 317 for DON, NIV, 3-ADON and 15-ADON, and ZEA, respectively.