应用Mycosep多功能净化柱液相色谱法测定农产品中黄曲霉毒素。

Thomas J Wilson, T. Romer
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引用次数: 50

摘要

建立了一种使用Mycosep多功能清除(MFC)柱的液相色谱(LC)技术。MFC柱提供快速的一步萃取纯化。它们被设计用来保留可能对分析方法产生干扰的特定化合物群。同时,MFC柱允许感兴趣的化合物通过。在本文提出的方法中,测试样品在含有乙腈-水(9 + 1)的搅拌器中提取。一部分提取物强制通过专门为分析多种真菌毒素而设计的MFC柱。当黄曲霉毒素通过色谱柱时,分析干扰被保留。将纯化提取物与水-三氟乙酸-乙酸(7 + 2 + 1)的混合物在65℃加热8.5 min,将黄曲霉毒素B1和G1转化为半缩醛。该混合物的等温液相色谱采用乙腈-水流动相和荧光检测进行分析。黄曲霉毒素B1的检出限小于0.5 ng/g。黄曲霉毒素(B1、B2、G1和G2)的平均回收率大于95%,变异系数小于3%。该方法成功地应用于以下商品:玉米、杏仁、开心果、核桃、花生、巴西坚果、米米、大米、棉籽、玉米粉、玉米蛋白粉、无花果膏和混合饲料。
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Use of the Mycosep multifunctional cleanup column for liquid chromatographic determination of aflatoxins in agricultural products.
A liquid chromatographic (LC) technique has been developed that uses the Mycosep multifunctional cleanup (MFC) column. MFC columns provide a rapid 1-step extract purification. They are designed to retain particular groups of compounds that may create interferences in analytical methods. At the same time, MFC columns allow compounds of interest to pass through. In the method presented, test samples are extracted in a blender with acetonitrile-water (9 + 1). A portion of the extract is forced through an MFC column designed especially for analysis of numerous mycotoxins. Analytical interferences are retained, while aflatoxins pass through the column. Aflatoxins B1 and G1 are converted to their hemiacetals by heating a mixture of purified extract and water-trifluoroacetic acid-acetic acid (7 + 2 + 1) at 65 degrees C for 8.5 min. An aliquot of this mixture is analyzed by isocratic LC with acetonitrile-water mobile phase and fluorescence detection. A detection limit of less than 0.5 ng/g for aflatoxin B1 was obtained. Average recoveries greater than 95% total aflatoxins (B1, B2, G1, and G2) and coefficients of variation of less than 3% were obtained. The method was successfully applied to the following commodities: corn, almonds, pista-chios, walnuts, peanuts, Brazil nuts, milo, rice, cottonseed, corn meal, corn gluten meal, fig paste, and mixed feeds.
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