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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 C_(18)柱(2.1 mm×100 mm,1.7μm)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0.1μg/kg,定量限为0.3μg/kg,线性范围为2.0~30.0μg/L;脱氧雪腐镰刀菌烯醇及其衍生物的检出限为0.2μg/kg,定量限为0.6μg/kg,线性范围为10.0~150.0μg/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。
Objective To establish deoxynivalenol (DON), 3-acetyl deoxidized snow-scylienol (3-AC-DON), 15-acetyl deoxy snow The determination of 15-acetyl deoxidized snow-scyloxanol (15-AC-DON) and zearalenone (ZEN) by ultra performance liquid chromatography-tandem triple quadrupole mass spectrometry. Methods Samples were extracted with acetonitrile - water (84:16, V: V) and purified by a multifunctional purification column. The mobile phase was separated on a BEH C 18 column (2.1 mm × 100 mm, 1.7 μm) Acetonitrile gradient elution, and multiple reaction monitoring (MRM) mode. Results The detection limit of zearalenone was 0.1μg / kg, the limit of quantification was 0.3μg / kg and the linear range was 2.0 ~ 30.0μg / L. The detection limit of deoxynivalenol and its derivatives was 0.2 μg / kg, the limit of quantification was 0.6μg / kg and the linear range was 10.0 ~ 150.0μg / L. Spike recovery of 88.9% ~ 106.0%. Conclusion The method is rapid, accurate and sensitive, and can meet the simultaneous detection of four kinds of Fusarium toxins.