First step in development and evaluation simultaneous determination of mycotoxins in cereals by liquid chromatography - mass spectrometry

Abstract

Currently, solid phase extraction (SPE) with immunoaffinity columns is applied in most standardized methods for mycotoxin determination to purify extracts and analysis by HPLC-FLD, HPLC-UV/VIS or LC-MS/MS. Therefore, sample preparation and analysis by instruments are time-consuming and high operating costs. The novel method allow simultaneously identify nine mycotoxin compounds with selective, stable and accurate results. The new method has been evaluated through three stages including validation as requirements of CEN/TR 16059:2010 (phase 1), comparison with current standard methods (phase 2), evaluate the method using an interlaboratory comparison program (phase 3).

Cereal samples were extracted by QuEChERS and analyzed by LC-MS/MS. The limit of quantitation (LOQ) was 0,5 μg/kg for each aflatoxin compound and 40 μg/kg, 25 μg/kg, 1 μg/kg, 75 μg/kg for deoxynivalenol, zearalenone, ochratoxin A, each toxin fumonisin (B1&B2), respectively. The recovery is in the range of 70-120%, relative standard deviation RSD < 20%. The novel method also gives the same results compared to the individual standardized methods, using the immunoaffinity column in the extraction stage. At the present, the method is being evaluated through an interlaboratory comparison program with two rounds: round 1 (for survey) and round 2 (official round), which is expected to be implemented in 2022.