Simultaneous analysis of multiple mycotoxins in Alpinia oxyphylla by UPLC-MS/MS

Abstract

In this study, a reliable and fast method for the simultaneous quantitation of 11 mycotoxins in Alpinia oxyphylla was developed using ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLCMS/ MS). Three different extraction procedures (solid-liquid extraction, solid-phase extraction and modified QuEChERS) were evaluated. Solid-liquid extraction was fast and easy, and also provided the best recovery rate for all mycotoxins, compared to the other extraction procedures. Some crucial factors, including extraction solvent, time and temperature, were carefully optimised. Significant matrix effects were offset using matrix-matched calibration. Under these optimised conditions, our detection approach showed a good, linear dynamic range with correlation coefficients (R2) above 0.9958. The limit of quantification ranged from 0.1 to 20 μg/kg. Accuracy was determined in a selected matrix using blank samples spiked with the target mycotoxins at three different concentration levels. The recoveries ranged from 60% (T-2 toxin) to 111% (HT-2 toxin), with relative standard deviation <20%. The validated method was used to analyse 44 batches of A. oxyphylla purchased from different regions of China. Aflatoxin B1, zearalenone, ochratoxin A, fumonisin B1 and fumonisin B2 were detected in 4 mouldy samples.