液液萃取-高效液相色谱法测定粮食中黄曲霉毒素的研究

Analysis of Aflatoxin in Grain by Liquid-Liquid Extraction-High Performance Liquid Chromatography

采用液液萃取净化的前处理方法,建立了用甲醇-乙腈-水（40∶5∶55体积比）三元流动相体系分离黄曲霉毒素（G2、G1、B2、B1）,柱后碘衍生、高效液相色谱荧光检测器测定粮食中黄曲霉毒素的新方法。使用该方法可在24 min内完成测定,4种黄曲霉毒素的线性关系r值均大于0.9995。样品在不同水平的加标回收试验中,回收率为80.3%~97.0%,相对标准偏差2.1%～4.0%,黄曲霉毒素G2、G1、B2、B1的检出限均小于0.40μg/kg。该方法具有样品前处理简单、操作稳定、试剂消耗少、成本低、准确且重复性好等优点,适用于粮食中黄曲霉毒素的定性定量分析。

A new method for aflatoxin G2, G1, B2 and B1 in grain by post-column derivatization with iodine and high performanceliquid chromatography-fluorescence detection was developed.Liquid-liquid extraction was used for sample cleanup and full sep- aration of 4 aflatoxins could be achieved by the mobile phase composed of methanol-acetonitrile-water （40：5：55, V/V） within 24 minutes. The average correlation of calibration curve was of 0.9995.Recoveries of samples at several spiked levels were ranged between 80.3 % and 97.0%, and the relative standard deviation （RSD） was 2.1%-4.0%. The limit of determination （LOD） of alia- toxins G2, G1, B2 and B1 were below 0.40μg/kg.This method has advantages of simple process of sample treatment,low consump- tion of reagents, low cost, rapid and exact, and is suitable for the quantitative and qualitative determination of aflatoxin in grain.