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目的建立光化学衍生-高效液相色谱荧光法测定粮谷类样品中的黄曲霉毒素(AFT)含量。方法样品经Romer Labs免疫亲和柱净化,经SW-3光化学柱后衍生,经高效液相色谱分离和荧光检测器测定,分析其中黄曲霉毒素B_1、B_2、G_1、G_2的含量。同时对免疫亲和柱洗脱条件、流动相的洗脱程序进行了优化。结果在0.5~10 ng/mL(AFT B_1,G_1)和0.15~3.0 ng/mL(AFT B_2,G_2)线性范围内,所得回归方程的相关系数均大于0.999。黄曲霉毒素B_1、G_1方法检出限为0.15 ng/g,黄曲霉毒素B_2、G_2方法检出限为0.05 ng/g,加标回收率为89.5%~107%,精密度为1.4%~7.2%。采集粮谷类样品222件,其中有5件样品检出AFT,但均未超过国家限值标准。结论该方法灵敏度和准确度较高,可适用于粮谷类食品中黄曲霉毒素的检测。
Objective To establish a method for the determination of aflatoxins (AFT) in grain and grain samples by photochemical derivatization - high performance liquid chromatography. Methods The samples were purified by Romer Labs immunoaffinity column and derivatized with SW-3 photochemical column. The contents of aflatoxins B 1, B 2, G 1 and G 2 were determined by HPLC and fluorescence detector. At the same time, the elution condition of immunoaffinity column and mobile phase were optimized. Results The correlation coefficient of the regression equation was greater than 0.999 in the linear range of 0.5 ~ 10 ng / mL (AFT B_1, G_1) and 0.15 ~ 3.0 ng / mL (AFT B_2, G_2). The detection limit of aflatoxins B_1 and G_1 was 0.15 ng / g, the detection limit of aflatoxin B_2 and G_2 was 0.05 ng / g, the recoveries were 89.5% -107% and the precision was 1.4% -7.2 %. A total of 222 grain samples were collected. Among them, 5 samples were tested for AFT but none of them exceeded the national limits. Conclusion The method has high sensitivity and accuracy and can be applied to the determination of aflatoxins in cereals.