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玉米粉尘中黄曲霉毒素的薄层色谱测定法。

Thin layer chromatographic determination of aflatoxin in corn dust.

作者信息

Shotwell O L, Burg W R, Diller T

出版信息

J Assoc Off Anal Chem. 1981 Sep;64(5):1060-3.

PMID:6793549
Abstract

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.

摘要

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。

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