Trucksess M W, Ready D W, Pender M K, Ligmond C A, Wood G E, Page S W
U.S. Food and Drug Administration, Center for Food Safety and Applied Nutrition, Division of Natural Products, Washington, DC 20204, USA.
J AOAC Int. 1996 Jul-Aug;79(4):883-7.
A liquid chromatographic (LC) method for determining deoxynivalenol (DON) in white flour, whole wheat flour, and bran was developed. A 25 g test portion was extracted with acetonitrile-water (84 + 16), and the extract was filtered and applied to a column containing a combination of charcoal, Celite, and other adsorbents. The eluate was then chromatographed on a silica-based, reversed-phase LC column by using a gradient of water and methanol. DON was measured at 220 nm. Average recoveries of DON from white flour, whole wheat flour, and bran spiked at 1 microgram/g were 88, 86, and 85%, respectively. The limit of determination of the method was < 0.5 micrograms/g. A total of 562 wheat-based products from the 1993 crop year were collected by 21 U.S. Food and Drug Administration District Offices and analyzed by this method in Kansas City, Seattle, and New Orleans District Laboratories. The numbers of samples with DON contamination > or = 1 microgram/g from 163 bran, 272 white flour, 90 whole wheat flour, and 37 miscellaneous test samples were 20, 28, 14, and 2, respectively. About 52, 50, 40, and 27% of the same test samples were contaminated with DON at levels > 0.01 micrograms/g.
建立了一种用于测定白面粉、全麦面粉和麸皮中脱氧雪腐镰刀菌烯醇（DON）的液相色谱（LC）方法。称取25 g试验份，用乙腈 - 水（84 + 16）萃取，萃取液过滤后加至装有活性炭、硅藻土及其他吸附剂组合的柱上。然后，洗脱液在硅胶基反相LC柱上进行色谱分析，采用水和甲醇梯度洗脱。在220 nm处测定DON。在白面粉、全麦面粉和麸皮中添加1 μg/g的DON，平均回收率分别为88%、86%和85%。该方法的测定限<0.5 μg/g。1993作物年度的562份小麦制品由美国食品药品管理局的21个地区办公室收集，并在堪萨斯城、西雅图和新奥尔良地区实验室采用该方法进行分析。在163份麸皮、272份白面粉、90份全麦面粉和37份其他试验样品中，DON污染水平≥1 μg/g的样品数量分别为20、28、14和2。相同试验样品中，DON污染水平>0.01 μg/g的分别约占52%、50%、40%和27%。
