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目的建立同时检测食品中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)和脱氧雪腐镰刀菌烯醇(DON)的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。方法采用Waters Acquity UPLC BEH C18色谱柱(1.7μm,50 mm×2.1 mm)、乙腈-0.1%氨水流动相、柱温35℃、质谱采用电喷雾电离(ESI)多反应监测(MRM)负离子模式进行检测,样品以乙腈-水为提取溶剂,经C18固体萃取吸附剂除去基质干扰,取10μl注入UPLC-MS/MS。结果 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)和脱氧雪腐镰刀菌烯醇(DON)在5~200μg/L范围内呈良好的线性关系,加标回收率在85.9%~109.8%,所测定的相对标准偏差在2.34%~5.20%之间。结论该方法灵敏、快速,经济,结果准确可靠,可为食品中4种真菌毒素检测提供可靠的分析方法。
Objective To establish a method for the simultaneous determination of 3-acetyl deoxynivalenol (3-ADON), 15-acetyl deoxynivalenol (15-ADON), snow rot Fusarium enolase (NIV) Method for the analysis of DON by UPLC-MS / MS. Methods A Waters Acquity UPLC BEH C18 column (1.7 μm, 50 mm × 2.1 mm) was used. The mobile phase was acetonitrile-0.1% aqueous ammonia. The column temperature was 35 ℃ and the mass spectrometry was performed by electrospray ionization (ESI) Detection, the sample with acetonitrile - water as the extraction solvent, the C18 solid extract adsorbent to remove matrix interference, take 10μl injection UPLC-MS / MS. Results 3-Acetyl deoxynivalenol (3-ADON), 15-acetyl deoxynivalenol (15-ADON), Fusarium venenatum enolase (NIV) and deoxynivalenol (DON) in the range of 5 ~ 200μg / L showed a good linearity with recoveries of 85.9% -109.8%. The relative standard deviations (RSDs) were between 2.34% and 5.20%. Conclusion The method is sensitive, rapid, economical and the results are accurate and reliable. It can provide a reliable analytical method for the detection of four mycotoxins in food.