Fast determination of multi-mycotoxins in corn by dispersive solid-phase extraction coupled with ultra-performance liquid chromatography with tandem quadrupole time-of-flight mass spectrometry

doi:10.1016/S2095-3119(15)61287-4

Journal of Integrative Agriculture ›› 2016, Vol. 15 ›› Issue (7): 1656-1666.DOI: 10.1016/S2095-3119(15)61287-4

Fast determination of multi-mycotoxins in corn by dispersive solid-phase extraction coupled with ultra-performance liquid chromatography with tandem quadrupole time-of-flight mass spectrometry

收稿日期:2015-11-02 出版日期:2016-07-06 发布日期:2016-07-06

Fast determination of multi-mycotoxins in corn by dispersive solid-phase extraction coupled with ultra-performance liquid chromatography with tandem quadrupole time-of-flight mass spectrometry

WANG Yan^{1, 2}, DONG Yan-jie¹, LI Zeng-mei¹, DENG Li-gang¹, GUO Chang-ying¹, ZHANG Shu-qiu¹, LI Da-peng², ZHAO Shan-cang¹

¹Institute of Agricultural Quality Standards and Testing Technology Research, Shandong Academy of Agricultural Sciences, Jinan 250100, P.R.China
² Academy of Food Science and Engineering, Shandong Agricultural University, Tai’an 271018, P.R.China

Received:2015-11-02 Online:2016-07-06 Published:2016-07-06
Contact: ZHAO Shan-cang, Tel: +86-531-83178203, Fax: +86-531-88960397, E-mail: shancangzhao@126.com
About author:WANG Yan, E-mail: wangyan891217@163.com
Supported by:
This study was supported by the Key Project of Science and Technology Development Program of Shandong Province, China (2013KF03).

摘要/Abstract

Abstract: A fast analytical method for the simultaneous determination of 9 mycotoxins, including aflatoxins (B₁, B₂, G₁, and G₂), fumonisins (B1, B2 and B3), zearalenone, and deoxynivalenol in corn using dispersive solid-phase extraction method and ultra-performance liquid chromatography coupled to tandem quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) was developed and validated. Samples were extracted with acetonitrile-water (84:16, v:v, containing 1% acetic acid) using ultrasonic extraction. The extracts were purified with a dispersive SPE method using C18 as a cleaning agent. The final clear extracts were dried by nitrogen blowing and subsequently redissolved in methanol-water (5:5, v:v). The samples were then analyzed by UPLC-Q-TOF-MS with 0.1% formic acid in ammonium acetate-methanol as mobile phase. The mean recoveries were ranged from 68.0 to 120.0%, and the relative standard deviation (RSD) ranged from 0.18 to 6.29%. Limits of detections ranged from 0.05 to 50 μg kg⁻¹, and limits of quantification ranged from 0.1 to 200 μg kg⁻¹, which were below the legal limits set by the European Union for the legislated mycotoxins. The developed method was applied to 130 corn samples. Among the mycotoxins studied, aflatoxins B₁ and fumonisins B₁, B₂ and B₃ were the most predominant mycotoxins, and their concentrations were 0–593.12, 0–2.01×10⁴, 0–6.94×10³ and 0–3.05×10³ µg kg^–1, respectively.

Key words: C18 , corn , mycotoxins , dispersive solid-phase extraction

WANG Yan, DONG Yan-jie, LI Zeng-mei, DENG Li-gang, GUO Chang-ying, ZHANG Shu-qiu, LI Dapeng, ZHAO Shan-cang. Fast determination of multi-mycotoxins in corn by dispersive solid-phase extraction coupled with ultra-performance liquid chromatography with tandem quadrupole time-of-flight mass spectrometry[J]. Journal of Integrative Agriculture, 2016, 15(7): 1656-1666.

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Fast determination of multi-mycotoxins in corn by dispersive solid-phase extraction coupled with ultra-performance liquid chromatography with tandem quadrupole time-of-flight mass spectrometry

Fast determination of multi-mycotoxins in corn by dispersive solid-phase extraction coupled with ultra-performance liquid chromatography with tandem quadrupole time-of-flight mass spectrometry

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