Tacke B K, Casper H H
Department of Veterinary and Microbiological Sciences, North Dakota State University, Fargo 58105, USA.
J AOAC Int. 1996 Mar-Apr;79(2):472-5.
A rapid and reliable method to determine deoxynivalenol (DON) in wheat, barley, and malt is described. Samples are extracted with acetonitrile-water (84 + 16). Extracts are eluted through a C18-alumina (1 + 3) column, evaporated to dryness, and derivatized with trimethylsilylimidazole-trimethylchlorosilane (100 + 1). DON is identified and quantitated by capillary gas chromatography with electron capture detection. This method can quantitate DON levels from 0.2 to 40 ppm. Multiple analyses of wheat spiked at 2 ppm and of naturally contaminated wheat, malt, and barley resulted in coefficients of variation of 5.1, 5.1, 6.0, and 9.8%, respectively. Recoveries of DON spikes at 3 levels were 94-100% for wheat, 100-105% for barley, and 100-105% for malt. Results for wheat sample analyzed with this procedure (1.9 +/- 0.1 ppm DON) compared well with results for the same sample analyzed by enzyme-linked immunosorbent assay (1.9 ppm DON) and by liquid chromatography (1.7 ppm DON).
本文描述了一种快速、可靠的检测小麦、大麦和麦芽中脱氧雪腐镰刀菌烯醇（DON）的方法。样品用乙腈 - 水（84 + 16）提取。提取物通过C18 - 氧化铝（1 + 3）柱洗脱，蒸发至干，并与三甲基硅咪唑 - 三甲基氯硅烷（100 + 1）衍生化。DON通过带有电子捕获检测的毛细管气相色谱法进行鉴定和定量。该方法可定量0.2至40 ppm的DON水平。对添加2 ppm DON的小麦以及天然污染的小麦、麦芽和大麦进行多次分析，变异系数分别为5.1%、5.1%、6.0%和9.8%。三个添加水平的DON回收率，小麦为94 - 100%，大麦为100 - 105%，麦芽为100 - 105%。用该方法分析的小麦样品结果（1.9±0.1 ppm DON）与用酶联免疫吸附测定法（1.9 ppm DON）和液相色谱法（1.7 ppm DON）分析的同一样品结果相比良好。
