Multi-walled carbon nanotubes-based magnetic solid-phase extraction for the determination of zearalenone and its derivatives in maize by ultra-high performance liquid chromatography-tandem mass spectrometry

- Synthesis of MWCNT-MNPs and approaches for their use in M-SPE.
- M-SPE was proposed for clean-up of zearalenone and its derivatives in maize.
- UHPLC-MS/MS detection combined with M-SPE purification for rapid analysis.
- Matrix effects were eliminated and matrix-matched calibration was unnecessary.
- The approach provides the desirable level of sensitivity, recovery and precision.

A simple and rapid magnetic solid-phase extraction (M-SPE) procedure using multi-walled carbon nanotube-magnetic nanoparticles (MWCNT-MNPs) as sorbents was established for purification of zearalenone (ZEA), α-zearalenol (α-ZOL), β-zearalenol (β-ZOL), zearalanone (ZAN), α-zearalanol (α-ZAL) and β-zearalanol (β-ZAL) in maize. The main parameters affecting the clean-up efficiency were thoroughly investigated, and high purification efficiencies for all analytes were obtained. The resulting MWCNT-MNP-ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was validated for maize samples. The matrix effects were greatly minimized using the M-SPE approach, with signal suppression/enhancement values decreased from 69.9-127.6% to 92.1-103.8%. Consequently, complex matrix-matched calibration curves were not necessary and the calibrations constructed in acetonitrile could be applied for accurate quantification of the targeted mycotoxins in real samples. The average recoveries ranged from 75.8 to 104.1% and the inter- and intra-day precision values expressed as RSDs, were all lower than 14%. Limits of detection and quantification were in the range of 0.03-0.04 and 0.07-0.10 μg/kg, respectively. The analytical performance of the developed method was also successfully evaluated with maize samples, and this method was proved to be a powerful tool for monitoring ZEA and its derivatives in maize.