Stack M E, Nesheim S, Brown N L, Pohland A E
J Assoc Off Anal Chem. 1976 Sep;59(5):966-70.
Corn and oats samples are extracted with acetonitrile-water, followed by partition of the extract against hexane, transfer to chloroform, and elution from a silica gel column. The extract is purified by gel permeation chromatography on an automatic instrument. Reverse phase high-pressure liquid chromatography, using a 254 nm ultraviolet detector and 0.1 M KH2PO4-acetonitrile (7+5) as the mobile phase, is used for quantitation. The average recovery from 6 samples of corn to which 0, 25, 50, and 100 mug sterigmatocystin/kg had been added was 59%, with a coefficient of variation of 8.4%. The average recovery from oats fortified at the same levels was 74%, with a coefficient of variation of 12%. A confirmation procedure based on hemiacetal derivative formation on a thin layer chromatographic plate is also described.
玉米和燕麦样品用乙腈 - 水萃取，接着将萃取液用正己烷分配，转移至氯仿中，并从硅胶柱上洗脱。萃取液在自动仪器上通过凝胶渗透色谱法进行纯化。使用254 nm紫外检测器，以0.1 M KH₂PO₄ - 乙腈（7 + 5）作为流动相的反相高压液相色谱法用于定量分析。向6份玉米样品中分别添加0、25、50和100 μg/kg的柄曲霉素，其平均回收率为59%，变异系数为8.4%。在相同添加水平下强化燕麦的平均回收率为74%，变异系数为12%。文中还描述了一种基于在薄层色谱板上形成半缩醛衍生物的确证方法。
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