关键词: 免疫亲和, 玉米赤霉烯酮, 超高效液相色谱-串联质谱, 食品中真菌毒素

Abstract: A method was established for the determination of 6 zeranols (α-zearalanol, β-zearalanol, α-zearalenol, β-zearalenol, zearalanone, and zearalenon) in foods by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with immunoaffinity column clean-up. Sample extraction was carried out with 80% (V/V) acetonitrile-water mixture followed by purification on an immunoaffinity column, which was eluted with 2 mL of acetonitrile, and the eluate was blown to dryness by nitrogen and redissolved with 0.5 mL of 50% (V/V) acetonitrile-water mixture. The target compounds were assayed by UPLC-MS/MS. The chromatographic separation was performed on an ACQUITY UPLC HSS T3 column by gradient elution using acetonitrile and water as mobile phase. The mass spectrometric acquisitions were carried out by means of multiple reaction monitoring (MRM) in the electrospray negative ionization mode. Good linearities (R2 > 0.992) were achieved for these 6 compounds over the concentration range of 0.1–100 μg/L. The limit of detection (LOD) of the method was 0.05 μg/kg, and the limit of quantification (LOQ) was 0.2 μg/kg. The mean recoveries of the 6 target compounds (spiked at three concentration levels) ranged from 73.0% to 119.1%, with relative standard deviations (RSDs) of not more than 10%. This method is suitable for the simultaneous determination of multiple zearalenonic mycotoxins in foods with simple pretreatment, high sensitivity, and good recovery.

Key words: immunoaffinity, zearalenon, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), mycotoxins in foods