Bao Lei, Oles Carolyn J, White Kevin D, Sapp Chelsea, Trucksess Mary W
U.S. Food and Drug Administration, Center for Food Safety and Applied Nutrition, Office of Regulatory Science, Division of Bioanalytical Chemisty, College Park, MD, USA.
J AOAC Int. 2011 Sep-Oct;94(5):1506-12. doi: 10.5740/jaoacint.10-477.
Deoxynivalenol (DON), also known as vomitoxin, belongs to a class of naturally occurring mycotoxins produced by Fusarium spp. DON, 12, 13-epoxy-3,7 trihydroxytrichothec-9-en-8-one, is one of the most frequently detected mycotoxins in agricultural commodities worldwide. A method consisting of extraction, filtration, column cleanup, and RP-HPLC-UV separation and quantitation was validated for the determination of DON in grains (rice and barley), grain products (whole wheat flour, white flour, wheat germ, and wheat bran), and processed foods (bread, breakfast cereals, and pretzels). A 25 g test portion was extracted with 100 mL acetonitrile-water (84 + 16, v/v). After blending for 3 min, the supernatant was applied to a multifunctional column (MycoSep 225). The purified filtrate (2 mL) was evaporated to dryness and redissolved in the mobile phase. The toxins were then subjected to RP-HPLC-UV analysis. The accuracy and repeatability characteristics of the method were determined. Recoveries of DON added at levels ranging from 0.5 to 1.5 microg/g for all test matrixes were from 75 to 98%. SD and RSD(r) ranged from 0.7 to 11.6% and 0.9 to 12.7%, respectively. Within-laboratory HorRat values were from 0.1 to 0.7 for all matrixes analyzed. The method was found to meet AOAC method performance criteria for grains, grain products, and processed foods. The identity of DON in naturally contaminated test sample extracts was confirmed by HPLC/MS/MS analysis.
脱氧雪腐镰刀菌烯醇（DON），又称呕吐毒素，属于镰刀菌属产生的一类天然存在的霉菌毒素。DON，即12,13 -环氧-3,7 -三羟基单端孢霉烯-9 -烯-8 -酮，是全球农产品中最常检测到的霉菌毒素之一。一种由萃取、过滤、柱净化以及反相高效液相色谱-紫外检测分离和定量组成的方法，被验证可用于测定谷物（大米和大麦）、谷物制品（全麦粉、白面粉、小麦胚芽和麦麸）以及加工食品（面包、早餐谷物和椒盐脆饼）中的DON。称取25 g测试份，用100 mL乙腈-水（84 + 16，v/v）萃取。搅拌3分钟后，将上清液加到多功能柱（MycoSep 225）上。将2 mL纯化后的滤液蒸发至干，再用流动相重新溶解。然后对毒素进行反相高效液相色谱-紫外分析。测定了该方法的准确性和重复性特征。所有测试基质中添加水平为0.5至1.5 μg/g的DON回收率为75%至98%。标准偏差（SD）和相对标准偏差（RSD(r)）分别为0.7%至11.6%和0.9%至12.7%。所有分析基质的实验室内HorRat值为0.1至0.7。该方法被发现符合美国官方分析化学师协会（AOAC）对谷物、谷物制品和加工食品的方法性能标准。通过高效液相色谱/串联质谱（HPLC/MS/MS）分析确认了天然污染测试样品提取物中DON的特性。
