Simultaneous determination of five Alternaria toxins in cereals using QuEChERS-based methodology

Publication date: 15 November 2017
Source:Journal of Chromatography B, Volumes 1068–1069
Author(s): Jian Zhou, Jiao-Jiao Xu, Zeng-Xuan Cai, Bai-Fen Huang, Mi-Cong Jin, Yi-Ping Ren
Two analytical approaches, including ultra-high performance liquid chromatograph linked with photo-diode array/fluorescence detector, and ultra-high performance liquid chromatography-tandem mass spectrometry, have been proposed for simultaneous determination of five Alternaria toxins in cereals, which both based on QuEChERS strategy. After QuEChERS extraction and salting out, the collected supernatant was subjected to an extra dispersive liquid–liquid microextraction step prior to quantitative analysis. Response surface methodology based on central composite design was employed to optimize the micro-extraction conditions. During photo-diode array/fluorescence detector method validation, satisfactory analytical characteristics, in terms of selectivity, recovery (72.7%–109.1%), precision (inter-day RSDs <9.6%), sensitivity (limits of quantification ranged from 2.1μgkg−1 to 120.0μgkg−1) and linearity (R2 all higher than 0.9984), were achieved. Mass spectrometry method was employed as a certified method for accuracy. The two methodologies were successfully applied to 71 samples including three different matrices and the quantitative results were compared. As the result of non-parametric test shown, the established two analytical approach exhibited comparable quantitative accuracy to each other.

Graphical abstract

image

Publication date: 15 November 2017
Source:Journal of Chromatography B, Volumes 1068–1069

Author(s): Jian Zhou, Jiao-Jiao Xu, Zeng-Xuan Cai, Bai-Fen Huang, Mi-Cong Jin, Yi-Ping Ren

Two analytical approaches, including ultra-high performance liquid chromatograph linked with photo-diode array/fluorescence detector, and ultra-high performance liquid chromatography-tandem mass spectrometry, have been proposed for simultaneous determination of five Alternaria toxins in cereals, which both based on QuEChERS strategy. After QuEChERS extraction and salting out, the collected supernatant was subjected to an extra dispersive liquid–liquid microextraction step prior to quantitative analysis. Response surface methodology based on central composite design was employed to optimize the micro-extraction conditions. During photo-diode array/fluorescence detector method validation, satisfactory analytical characteristics, in terms of selectivity, recovery (72.7%–109.1%), precision (inter-day RSDs <9.6%), sensitivity (limits of quantification ranged from 2.1μgkg−1 to 120.0μgkg−1) and linearity (R2 all higher than 0.9984), were achieved. Mass spectrometry method was employed as a certified method for accuracy. The two methodologies were successfully applied to 71 samples including three different matrices and the quantitative results were compared. As the result of non-parametric test shown, the established two analytical approach exhibited comparable quantitative accuracy to each other.

Graphical abstract

image