Romer T R, Boling T M, MacDonald J L
J Assoc Off Anal Chem. 1978 Jul;61(4):801-8.
A gas-liquid chromatographic method has been developed for the simultaneous determination of the T-2 toxin and diacetoxyscirpenol (DAS) in corn and mixed feeds. The analytes are extracted with aqueous methanol. Ammonium sulfate is used to denature and precipitate proteinaceous compounds and to salt out low polar compounds. The analytes are selectively concentrated into chloroform, which is washed with aqueous potassium hydroxide to remove acidic compounds. Residual interferences are removed by silica gel column chromatography. Heptafluorobutrylimidazole (HFBI) is added to form esters of the analytes. The HFB-esters are separated on an SE-30 glass column and measured witha 63Ni electron capture detector, using methoxychlor as an internal standard. The method has been applied to corn, livestock feeds, and pet food. The limit of detection is 100 ng T-2 toxin and 25 ng DAS/G. Average recoveries of 105 and 97% and coefficients of variation of 17 and 10% were obtained for T-2 toxin and DAS, respectively.
已开发出一种气相色谱法，用于同时测定玉米和混合饲料中的T-2毒素和二乙酰基麦角甾醇（DAS）。分析物用甲醇水溶液提取。硫酸铵用于使蛋白质化合物变性和沉淀，并盐析低极性化合物。分析物被选择性地浓缩到氯仿中，氯仿用氢氧化钾水溶液洗涤以除去酸性化合物。通过硅胶柱色谱法去除残留干扰。加入七氟丁酰咪唑（HFBI）以形成分析物的酯。HFB-酯在SE-30玻璃柱上分离，并用63Ni电子捕获检测器测量，以甲氧滴滴涕作为内标。该方法已应用于玉米、家畜饲料和宠物食品。检测限为100 ng T-2毒素和25 ng DAS/G。T-2毒素和DAS的平均回收率分别为105%和97%，变异系数分别为17%和10%。
