建立固相萃取-高效液相色谱对小麦中脱氧雪腐镰刀菌烯醇(deoxynivalenol,DON)进行测定的方法。从提取溶剂、净化方式、流动相组成以及流动相流速等条件优化DON检测方法。结果表明,当样品提取溶剂为乙腈-水(84∶16,V/V),Bond Elut Mycotoxin固相萃取柱净化,流动相组成为乙腈-水(6∶94,V/V),流速为0.9 m L/min时,DON检测结果最好,该检测方法的DON回收率达到90.12%~106.25%,日内和日间相对标准偏差分别为4.51%和6.12%。该方法快速、准确,重复性好,稳定性高,适合DON污染小麦样品的大批量检测。
Deoxynivalenol(DON) is a ubiquitous mycotoxin present in cereal grains such as wheat and corn. This mycotoxin causes huge damage to human and animal health. This study optimized the experimental conditions including extraction solvent, cleanup column, composition and flow rate of mobile phase for DON detection by high-performance liquid chromatography(HPLC) after solid-phase extraction(SPE) cleanup. The optimized HPLC method was established when the extraction was performed using a mixture of acetonitrile(ACN) and water(84:16, V/V) followed by SPE cleanup on a Bond Elut Mycotoxin column using a mobile phase consisting of ACN and water(6:94, V/V) at a flow rate of 0.9 m L/min. Under these conditions, the recoveries of DON with this method ranged from 90.12% to 106.25%, with intra- and inter-day relative standard deviations between 4.51% and 6.12%, respectively. The proposed method is applicable to determine DON in grains because of its rapidity as well as good accuracy, repeatability and stability.