Childress W L, Krull I S, Selavka C M
U.S. Food and Drug Administration, Winchester, Massachusetts 01890.
J Chromatogr Sci. 1990 Feb;28(2):76-82. doi: 10.1093/chromsci/28.2.76.
Deoxynivalenol (DON, vomitoxin) is a naturally occurring toxic fungal metabolite found in grains such as wheat, corn, rye, and barley. Current methods of analysis for DON and related trichothecene mycotoxins involve gas chromatography with electron capture detection, thin-layer chromatography, and high-performance liquid chromatography with ultraviolet detection. Improved sensitivity and selectivity for DON, as well as for the related compounds nivalenol and fusarenon-X, are made possible by the use of high-performance liquid chromatography with online, postcolumn photolysis and oxidative amperometric detection (HPLC-hv-EC). Conditions are optimized with respect to residence time in the photolytic reactor, applied potentials, mobile phase pH, and chromatographic parameters for the separation of DON, nivalenol, and fusarenon-X, and the technique is found to be linear over a range of 10 ppb-2 ppm with minimum detection limits on the order of 1-2 ng on-column (10-20 ppb). Since these compounds are not electroactive in the absence of photolysis, an additional mode of specificity is realized in addition to the chromatographic retention time and the dual-electrode response ratio. Some market samples of wheat naturally contaminated with DON are analyzed by this method, and the results are in agreement with those obtained by HPLC-UV and TLC analyses of the same samples.
脱氧雪腐镰刀菌烯醇（DON，呕吐毒素）是一种天然存在的有毒真菌代谢产物，存在于小麦、玉米、黑麦和大麦等谷物中。目前分析DON及相关单端孢霉烯族霉菌毒素的方法包括气相色谱-电子捕获检测法、薄层色谱法以及高效液相色谱-紫外检测法。采用带在线柱后光解和氧化安培检测的高效液相色谱法（HPLC-hv-EC），可提高对DON以及相关化合物雪腐镰刀菌烯醇和镰刀菌烯酮-X的灵敏度和选择性。针对光解反应器中的停留时间、施加电位、流动相pH值以及分离DON、雪腐镰刀菌烯醇和镰刀菌烯酮-X的色谱参数进行了优化，该技术在10 ppb - 2 ppm范围内呈线性，柱上最低检测限约为1 - 2 ng（10 - 20 ppb）。由于这些化合物在无光解时无电活性，除了色谱保留时间和双电极响应比外，还实现了另一种特异性模式。用该方法分析了一些天然受DON污染的小麦市场样品，结果与对相同样品进行HPLC-UV和TLC分析所得结果一致。
