Design of a combined microextraction and back-extraction technique for the analysis of mycotoxins in amaranth seeds

Abstract

Abstract A methodology was optimized for the determination of the mycotoxins deoxynivalenol and zearalenone in Amaranthus-based samples. The extraction/preconcentration procedure consisted of an in-phase liquid-liquid microextraction based on the solidification of a floating organic drop followed by a double solvent-assisted back-extraction combined with liquid chromatography-tandem mass spectrometry (DLLME-SFO-SBE). The solvent assisted back-extraction enabled the direct injection of deoxynivalenol (DON) and zearalenone (ZEA) in the ultra-high performance liquid chromatography-tandem mass spectrometry system configured with an electrospray source operated in a positive polarity mode (UHPLC-ESI+-MS/MS). Parameters affecting the efficiency of the back-extraction procedure were evaluated and optimized, including the nature of the back-extractant volume and the agitation effect. Detection and quantification limits were in the range of 0.07−0.73\u2009μg kg−1 and 0.22−0.91\u2009μg kg−1. Acceptable extraction recoveries between 80.35 and 100.05 % and enrichment factors between 16 and 20-fold, with relative standard deviations