UHPLC-ToF-MS method for determination of multi-mycotoxins in maize: Development and validation

Ana Sanches Silva; Carla Brites; Ana Vila Pouca; Jorge Barbosa; Andreia Freitas

doi:10.1016/j.crfs.2019.07.001

UHPLC-ToF-MS method for determination of multi-mycotoxins in maize: Development and validation

Curr Res Food Sci. 2019 Jul 31:1:1-7. doi: 10.1016/j.crfs.2019.07.001. eCollection 2019 Nov.

Authors

Ana Sanches Silva^{1

2}, Carla Brites^{1

3}, Ana Vila Pouca¹, Jorge Barbosa^{1

4}, Andreia Freitas^{1

4}

Affiliations

¹ National Institute for Agricultural and Veterinary Research (INIAV), Rua dos Lágidos, Lugar da Madalena, 4485-655 Vila do Conde, Portugal.
² Center for Study in Animal Science (CECA), ICETA, University of Oporto, Oporto, Portugal.
³ GREEN-IT, ITQB NOVA, Av. da República, 2780-157 Oeiras, Portugal.
⁴ REQUIMTE/ LAQV, Pharmacy Faculty, University of Coimbra, Azinhaga de Santa Comba, 3000-548 Coimbra, Portugal.

Abstract

An Ultra-High Performance Liquid Chromatography combined with Time-of-Flight Mass Spectrometry (UHPLC-ToF-MS) method has been developed for determination of nine mycotoxins, namely aflatoxins (AFB₁, AFB₂, AFG₁ and AFG₂), ochratoxin A (OTA), zearalenone (ZEA), toxin T2 (T2) and fumonisins (FB₁ and FB₂) in maize. The method included a two-step extraction with acetonitrile 80% (v/v). After optimization, the analytical method was validated. The different concentrations tested take in account the Maximum Levels (ML) for maize (Commission Regulation EC no. 1881/2006) and good results for repeatability (%RSD_r ≤ 15.4%), reproducibility (%RSD_R ≤ 15.9%) and recovery (77.8-110.4%, except for AFG2 at 2 μg/kg which presented a recovery of 73.4%) were achieved. These met the performance criteria imposed by Commission Regulation (EC) no. 401/2006. The method was applied to twenty-two samples from Portuguese producers of maize. Fumonisins were the most frequently detected mycotoxins, but the levels do not exceed those imposed by European legislation.

Keywords: Cereals; Maize; Mycotoxins; Time-of-flight mass spectrometry; Ultra-high performance liquid chromatography; Validation.