Rood H D, Buck W B, Swanson S P
University of Illinois, Department of Veterinary Biosciences, Urbana 61801.
J Assoc Off Anal Chem. 1988 May-Jun;71(3):493-8.
A gas chromatographic method for screening trichothecene mycotoxins in feeds is described. Feed is extracted with acetonitrile-water, and the toxins are purified with charcoal-alumina-Celite, Florisil, and silica mini-columns. Deoxynivalenol (DON), nivalenol (NIV), diacetoxyscirpenol (DAS), T-2 toxin, and their fungal metabolites are hydrolyzed to their corresponding parent alcohols (DON, NIV, scirpentriol, or T-2 tetraol) by alkaline hydrolysis. After derivatization to their pentafluoropropionyl analogs, they are quantitated by capillary gas chromatography with electron capture detection. Identity can be confirmed and sensitivity can be increased by using negative chemical ionization mass spectrometry with no additional sample workup. Recoveries of DAS, DON, and T-2 toxin averaged, respectively, 80, 65, and 85% in corn; 84, 65, and 88% in soybeans; and 70, 57, and 96% in mixed feeds at concentrations ranging from 0.1 to 2.0 ppm. Recoveries of 15-monoacetoxyscirpenol (MAS), HT-2, NIV, and T-2 tetraol were 97, 97, 86, and 56%, respectively, in corn at a concentration of 0.25 ppm: A detection limit of 0.02 ppm in corn, soybeans, and mixed feeds, and 0.05 ppm in silages is estimated.
本文描述了一种用于筛查饲料中单端孢霉烯族霉菌毒素的气相色谱方法。饲料用乙腈 - 水进行萃取，毒素通过活性炭 - 氧化铝 - 硅藻土、弗罗里硅土和硅胶微型柱进行纯化。脱氧雪腐镰刀菌烯醇（DON）、雪腐镰刀菌烯醇（NIV）、二醋酸雪腐镰刀菌烯醇（DAS）、T - 2毒素及其真菌代谢产物通过碱性水解被水解为相应的母体醇（DON、NIV、蛇形菌素或T - 2四醇）。在衍生化为其五氟丙酰类似物后，通过带有电子捕获检测的毛细管气相色谱法进行定量。通过使用负离子化学电离质谱法，无需额外的样品前处理即可确认其身份并提高灵敏度。在浓度范围为0.1至2.0 ppm时，玉米中DAS、DON和T - 2毒素的回收率分别平均为80%、65%和85%；大豆中分别为84%、65%和88%；混合饲料中分别为70%、57%和96%。在浓度为0.25 ppm的玉米中，15 - 单醋酸雪腐镰刀菌烯醇（MAS）、HT - 2、NIV和T - 2四醇的回收率分别为97%、97%、86%和56%。估计玉米、大豆和混合饲料中的检测限为0.02 ppm，青贮饲料中的检测限为0.05 ppm。
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