超高效液相色谱-串联质谱法检测小米及面粉中4种镰刀菌毒素

Determination of 4 Fusarium toxins in millet and flour by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  脱氧雪腐镰刀菌烯醇  3-乙酰脱氧雪腐镰刀菌烯醇  15-乙酰脱氧雪腐镰刀菌烯醇  玉米赤霉烯酮  面粉  小米

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  deoxynivalenol  3-acetyl deoxidized snow-scylienol  15-acetyl deoxidized snow-scyloxanol  zearalenone  flour  millet

中文摘要:

      目的 建立小米及面粉中脱氧雪腐镰刀菌烯醇(deoxynivalenol, DON)、3-乙酰脱氧雪腐镰刀菌烯醇(3-acetyl deoxidized snow-scylienol, 3-AC-DON)、15-乙酰脱氧雪腐镰刀菌烯醇(15-acetyl deoxidized snow -scyloxanol, 15-AC-DON)和玉米赤霉烯酮(zearalenone, ZEN)的超高效液相色谱-串联三重四极杆质谱测定方法。方法 经乙腈-水(84:16, V:V)提取样品, 通过多功能净化柱净化, 以BEH C18柱(2.1 mm×100 mm, 1.7 μm)分离, 流动相为0.2%氨水:乙腈梯度洗脱, 电喷雾离子(multiple reaction monitoring, MRM)模式检测。结果 玉米赤霉烯酮检出限为0.1 μg/kg, 定量限为0.3 μg/kg, 线性范围为2.0~30.0 μg/L ; 脱氧雪腐镰刀菌烯醇及其衍生物的检出限为0.2 μg/kg, 定量限为0.6 μg/kg, 线性范围为10.0~150.0 μg/L。加标回收率88.9%~106.0%。结论 本方法快速、准确、灵敏度高, 能满足4种镰刀菌毒素的同时检测。

英文摘要:

      Objective To establish a method for determination of deoxynivalenol (DON), 3-acetyl deoxidized snow-scylienol (3-AC-DON), 15-acetyl deoxidized snow–scyloxanol (15-AC-DON) and zearalenone(ZEN) in millet and flour using ultra performance liquid chromatography-triple quadruple tandem mass spectrometry (UPLC-MS/MS). Methods Samples were extracted using acetonitrile/H2O (84:16, V:V), and the extracts were purified by multifunction purification column. Substances were separated on a BEH C18 column (2.1 mm×100 mm, 1.7 μm) with a mobile phase composed of 0.2% ammonia and acetonitrile. The analysis was carried out with an eletrospray positive ion multiple reaction monitoring (MRM) mode. Results The linear range of ZEN was 2.0~30.0 μg/L and the limit of detection was 0.1 μg/kg, the limit of quantitation was 0.3 μg/kg. The linear ranges of DON, 3-Ac-DON and 15-Ac-DON were 10.0~150.0 μg/L and the limits of detection were 0.2 μg/kg, the limits of quantitation were 0.6 μg/kg. The recoveries were 88.9%~106.0%. Conclusion This method is rapid, accurate and sensitive, which can meet the requirements for the simultaneous determination of 4 Fusarium toxins.