Comprehensive assessment of different extraction methodologies for optimization and validation of an analytical multi-method for determination of emerging and regulated mycotoxins in maize by UHPLC-MS/MS

Abstract

A multi-analyte method for identification and quantification of 23 regulated and emerging mycotoxins was developed in maize samples by ultra high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Several extraction methodologies were evaluated, including solid-liquid extraction (SLE), solid-phase extraction (SPE), and modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) protocols. The final method consisting of an extraction by QuEChERS using C18 sorbents, was in-house validated in terms of linearity, repeatability, reproducibility, recovery, Limits of Detection (LOD) and Limits of Quantification (LOQ). Acceptable performance characteristics were obtained according to specific and general European regulations for regulated and emerging mycotoxins, respectively. The developed method proved to be specific and selective for all mycotoxins, with LODs and LOQs lower than 21.10 and 37.49 ng g−1, respectively; and recoveries ranging from 55.25 to 129.48% with precisions, expressed as relative standard deviations, below 15.03%. The method was successfully applied to real maize samples.

Keywords

• Mycotoxins
• Maize
• Solid-liquid extraction
• Solid phase extraction
• QuEChERS
• UHPLC-MS/MS