National Institute of Health Sciences, 1-18-1, Kamiyoga, Setagaya-ku, Tokyo 158-8501, Japan.
J Food Prot. 2012 Jul;75(7):1355-8. doi: 10.4315/0362-028X.JFP-11-555.
We developed a purification method based on liquid chromatography-tandem mass spectrometry for the identification of deoxynivalenol (DON), its acetylated derivatives (3-acetyl-deoxynivalenol and 15-acetyl-deoxynivalenol), and a glycosylated derivative (deoxynivalenol-3-glucoside [D3G]) in corn-based products. The analytes were extracted from samples with acetonitrile-water (85:15, vol/vol) and then purified with multifunctional columns. Evaluation of five kinds of multifunctional columns revealed that DON and its acetylated derivatives were recovered well (96 to 120%) by all columns, but D3G was recovered adequately (93.5%) by only one column, InertSep VRA-3. Samples of corn grits and corn flour were analyzed using the purification method with InertSep VRA-3. DON, D3G, and 15-acetyl-deoxynivalenol were the major contaminants in the samples harvested in 2009, but only DON was detected in the samples harvested in 2010. These results suggest that the purification method using InertSep VRA-3 is effective for identification of DON and its derivatives in corn-based products.
我们开发了一种基于液相色谱-串联质谱的净化方法，用于鉴定玉米制品中的脱氧雪腐镰刀菌烯醇（DON）、其乙酰化衍生物（3-乙酰基脱氧雪腐镰刀菌烯醇和 15-乙酰基脱氧雪腐镰刀菌烯醇）和一种糖化衍生物（脱氧雪腐镰刀菌烯醇-3-葡萄糖苷[D3G]）。分析物用乙腈-水（85:15，体积/体积）从样品中提取，然后用多功能柱进行净化。对五种多功能柱的评价表明，所有柱都能很好地回收 DON 和其乙酰化衍生物（96%至 120%），但只有 InertSep VRA-3 柱能充分回收 D3G（93.5%）。使用 InertSep VRA-3 柱对玉米粗粉和玉米粉样品进行了净化分析。2009 年收获的样品中主要污染物为 DON、D3G 和 15-乙酰基脱氧雪腐镰刀菌烯醇，但 2010 年收获的样品中仅检测到 DON。这些结果表明，使用 InertSep VRA-3 的净化方法可有效鉴定玉米制品中的 DON 及其衍生物。
