Shotwell O L, Burg W R, Diller T
J Assoc Off Anal Chem. 1981 Sep;64(5):1060-3.
Methods adopted by the AOAC and the American Association of Cereal Chemists for determining aflatoxin in corn were modified, and techniques were developed for application to samples of less than 1 to 10 g instead of the specified 50 g samples. Analysis included chloroform extraction of dust samples or dust collected from glass fiber filters, purification of extracts on a silica gel column of appropriate size, and measurement of aflatoxin by either 1- or 2-dimensional thin layer chromatography (TLC). The solvent for 1-dimensional TLC was chloroform-acetone-water (91 + 9 + 1). Solvents for 2-dimensional TLC were, first direction, ether-methanol-water (95 + 4 + 1, lined tank) and second direction, chloroform-acetone-water (91 + 9 + 1, unlined tank), or first direction, chloroform-acetone-water (91 + 9 + 1, unlined tank) and second direction, toluene-ethyl acetate-formic acid (60 + 30 + 10, unlined tank). When samples weighed less than or equal to 0.1 g, the entire concentrated extract was applied to the TLC plate. About 0.5-1.0 ng aflatoxin B1 could be detected on the plate, making the limit of detection about 9 ng/g for 0.1 g samples.
美国官方分析化学家协会(AOAC)和美国谷物化学家协会采用的测定玉米中黄曲霉毒素的方法被修改,并开发了适用于重量小于1至10克而非规定的50克样品的技术。分析包括对粉尘样品或从玻璃纤维滤器收集的粉尘进行氯仿萃取,在适当尺寸的硅胶柱上对萃取物进行纯化,以及通过一维或二维薄层色谱法(TLC)测定黄曲霉毒素。一维TLC的溶剂为氯仿 - 丙酮 - 水(91 + 9 + 1)。二维TLC的溶剂,第一方向为乙醚 - 甲醇 - 水(95 + 4 + 1,衬有内衬的展开槽),第二方向为氯仿 - 丙酮 - 水(91 + 9 + 1,无内衬的展开槽);或者第一方向为氯仿 - 丙酮 - 水(91 + 9 + 1,无内衬的展开槽),第二方向为甲苯 - 乙酸乙酯 - 甲酸(60 + 30 + 10,无内衬的展开槽)。当样品重量小于或等于0.1克时,将整个浓缩萃取物点样于TLC板上。在板上可检测到约0.5 - 1.0纳克黄曲霉毒素B1,对于0.1克样品,检测限约为9纳克/克。