超高效液相色谱串联质谱法测定面制品中脱氧雪腐镰刀菌烯醇及其衍生物的优化研究

Optimization of detection method for deoxynivalenol and its derivatives in flour products by ultra performance liquid chromatography coupled tandem mass spectrometry

目的优化改进超高效液相色谱串联质谱(UPLC-MS/MS)测定面制品中脱氧雪腐镰刀菌烯醇(DON)及其衍生物方法。方法样品经研磨粉碎,振荡提取后,过多功能柱净化,氮吹后复溶,对比不同阶段加入内标的测定结果,优化梯度洗脱条件和质谱条件。结果提取后加入内标操作更为简单节省,标准物质和加标样品测定结果满足分析要求,3种真菌毒素在2.0~1 000μg/L质量浓度范围内线性关系良好,相关系数r≥0.999 0,检出限范围为2.0~3.1μg/kg,回收率为91.9%~96.6%,相对标准偏差(RSD)为1.9%~4.8%。结论建立的方法快捷经济,准确可靠,适用于大批量面制品中DON及其衍生物的快速测定。

Objective To optimize and improve the detection method for deoxynivalenol(DON)and its derivatives in flour products by ultra high performance liquid chromatography coupled tandem mass spectrometry(UPLC-MS/MS).Methods The samples were grinded and comminuted,purified by multi-functional column after vortexing extraction,and dissolved again after nitrogen blowing.Compared with the results of internal standard added in different stages,the gradient elution condition and mass spectrometry condition were optimized.Results Adding internal standard after extraction was more simple and cost saving.The determination results of reference materials and spiked samples met the analysis requirements,The linear relationships of the3 mycotoxins were good in the range of 2.0-1 000μg/L,the correlation coefficients were≥0.9990,the detection limits were 2.0-3.1μg/kg,the recovery rates were 91.9%-96.6%,and the RSDs were 1.9%-4.8%.Conclusion The established method is fast,economic,accurate and reliable,whch is suitable for the rapid determination of Don and its derivatives in large quantities of flour products.