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目的建立同时测定食品中的脱氧雪腐镰刀菌烯醇(DON)、3-乙酰脱氧雪腐镰刀菌烯醇(3-ADON)、15-乙酰脱氧雪腐镰刀菌烯醇(15-ADON)、雪腐镰刀菌烯醇(NIV)、镰刀菌烯酮(Fus X)等B类单端孢烯霉族类真菌毒素的超高效液相色谱-串联质谱方法。方法样品经乙腈-水(84+16)溶液浸泡超声提取、227净化柱净化后,以水(A)和乙腈(B)为流动相经BEH C18柱(2.1 mm×100 mm,1.7μm)梯度洗脱分离,串联四级杆质谱在电喷雾负离子(ESI-)模式下同时测定。结果该法线性范围:DON、3-ADON、15-ADON、Fus X、NIV 5 ng/ml~900 ng/ml,r≥0.995,平均加标回收率75.2%~90.9%,精密度为3.4%~6.5%。结论本法灵敏度高、线性范围宽、结果准确可靠,可用于食品中的DON、3-ADON、15-ADON、NIV、Fus X的同时测定及确证。
Objective To establish a method for simultaneous determination of deoxynivalenol (DON), 3-acetyl deoxynivalenol (3-ADON), 15-ADOX deoxynivalenol (15-ADON) Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry Methods for Class B Monouppouse Mycotoxins Mycotoxins such as NIV, Fus X and so on. Methods The samples were extracted by soaking in acetonitrile - water (84 + 16) solution. After purification by 227 column, the gradient of BEA C18 column (2.1 mm × 100 mm, 1.7 μm) with water (A) and acetonitrile Elution separation, tandem quadrupole mass spectrometry in electrospray negative ion (ESI-) mode simultaneous determination. Results The linear range of this method was: DON, 3-ADON, 15-ADON, Fus X, NIV 5 ng / ml ~ 900 ng / ml and r≥0.995 with the average recovery of 75.2% ~ 90.9% and the precision of 3.4% ~ 6.5%. Conclusion This method has high sensitivity, wide linear range and accurate and reliable results. It can be used for the simultaneous determination and confirmation of DON, 3-ADON, 15-ADON, NIV and Fus X in food.