Pons W A
J Assoc Off Anal Chem. 1979 May;62(3):586-94.
A high pressure liquid chromatographic (HPLC) method is proposed for determining aflatoxins in corn. The sample is extracted with methanol-10% NaCl (4 + 1), pigments are precipitated with zinc acetate, and the extract is cleaned up on a small (2 g) silica gel column. Aflatoxins in the purified extract are resolved by normal phase HPLC on a microparticulate (10 micrometer) silica gel column with water-saturated chloroform-cyclohexane, acetonitrile solvent, and detected by fluorescence on a silica gel-packed flowcell. The method was compared with chloroform-water extraction of the official CB method on 15 samples of contaminated corn. In 5 of the 6 samples containing aflatoxins B1, B2, G1, and G2, methanol-10% NaCl extracted more aflatoxin than did cloroform-water, as measured both by HPLC and by thin layer chromatography. In samples containing only B1 and B2, the 2 extraction solvents were virtually equivalent. Agreement was good between HPLC and TLC for each extraction solvent. Average recovery of aflatoxins B1, B2, G1, and G2 added to yellow cornmeal at 3 levels was greater than 90%.
本文提出了一种用于测定玉米中黄曲霉毒素的高压液相色谱（HPLC）方法。样品用甲醇 - 10%氯化钠（4 + 1）萃取，色素用醋酸锌沉淀，萃取液在小型（2 g）硅胶柱上进行净化处理。纯化萃取液中的黄曲霉毒素通过正相HPLC在微粒（10微米）硅胶柱上，以水饱和氯仿 - 环己烷、乙腈为溶剂进行分离，并在硅胶填充流通池中通过荧光检测。该方法与官方CB方法的氯仿 - 水萃取法在15个受污染玉米样品上进行了比较。在含有黄曲霉毒素B1、B2、G1和G2的6个样品中的5个中，通过HPLC和薄层色谱法测定，甲醇 - 10%氯化钠萃取的黄曲霉毒素比氯仿 - 水更多。在仅含有B1和B2的样品中，两种萃取溶剂实际上相当。每种萃取溶剂的HPLC和TLC之间的一致性良好。向黄玉米粉中添加3种水平的黄曲霉毒素B1、B2、G1和G2的平均回收率大于90%。
