Trucksess M W, Nesheim S, Eppley R M
J Assoc Off Anal Chem. 1984 Jan-Feb;67(1):40-3.
A thin layer chromatographic (TLC) method for determining deoxynivalenol (DON) in corn and wheat was developed. DON is extracted from the grain with acetonitrile-water (84 + 16) and filtered through a column of mixed alumina-charcoal-Celite (0.5 g + 0.7 g + 0.3 g). The solvent is evaporated on a steam bath. Ethyl acetate is added to the residue and heated to dissolve DON. After cooling, the residue is transferred to a vial with additional ethyl acetate and is dissolved in CHCl3-acetonitrile (4 + 1) for TLC on an AlCl3-impregnated silica gel plate with CHCl3-acetone-isopropanol (8 + 1 + 1). The plate is heated in a 120 degrees C oven for 7 min; a blue fluorescent spot is produced under longwave ultraviolet light. DON is quantitated visually and/or fluorodensitometrically by comparison with reference standards. The minimum detectable amount of DON is ca 20 ng/spot. The limit of DON determination is ca 40 ng/g for wheat and 100 ng/g for corn. Recoveries of DON added to wheat and corn at 100, 500, and 1000 ng/g levels were 85, 93, and 88% and 77, 80, and 80%, respectively.
建立了一种用于测定玉米和小麦中脱氧雪腐镰刀菌烯醇(DON)的薄层色谱(TLC)方法。用乙腈 - 水(84 + 16)从谷物中提取DON,并通过混合氧化铝 - 木炭 - 硅藻土柱(0.5 g + 0.7 g + 0.3 g)过滤。溶剂在蒸汽浴上蒸发。向残渣中加入乙酸乙酯并加热以溶解DON。冷却后,将残渣转移至装有额外乙酸乙酯的小瓶中,并溶解于三氯甲烷 - 乙腈(4 + 1)中,在涂有三氯化铝的硅胶板上用三氯甲烷 - 丙酮 - 异丙醇(8 + 1 + 1)进行TLC分析。将板在120℃烘箱中加热7分钟;在长波紫外光下产生蓝色荧光斑点。通过与参考标准品比较,目视和/或荧光密度法对DON进行定量。DON的最低检测量约为20 ng/斑点。小麦中DON的测定限约为40 ng/g,玉米中为100 ng/g。在小麦和玉米中添加水平为100、500和1000 ng/g的DON的回收率分别为85%、93%和88%以及77%、80%和80%。