全自动固相萃取-HPLC-FLD柱后衍生法测定粮食中黄曲霉毒素B_(1)

Determination of Aflatoxin B_(1) in Grain by Automatic Solid Phase Extraction with HPLC-FLD Post-Column Derivatization

采用全自动固相萃取仪,建立适用于粮食中黄曲霉毒素B_(1)的检验方法。样品经提取液提取,用全自动固相萃取-免疫亲和柱净化,采用高效液相色谱-荧光检测(High Performance Liquid Chromatography-Fraunhofer Line Discriminator,HPLC-FLD)柱后衍生法进行测定。结果表明,黄曲霉毒素B_(1)在0.1~20.0 ng·mL^(-1)线性良好,R^(2)为0.999 987;检出限和定量限分别为0.03 μg·kg^(-1)和0.1 μg·kg^(-1);3水平加标回收率为84.9%~88.5%。本方法自动化程度高、重现性好,可以满足粮食中黄曲霉毒素B_(1)测定的要求。

A fully automatic solid-phase extractor was used to establish a method for the detection of aflatoxin B_(1) in grain.The samples were extracted by extraction,cleaned up with automatic solid-phase extraction-immunoaffinity column,and determined by high performance liquid chromatography-fraunhofer line discriminator (HPLC-FLD) post-column derivatization.The results showed that aflatoxin B_(1) had good linearity at 0.1~20.0 ng·mL^(-1),R^(2) was0.999 987,and the limits of detection and quantification were 0.03 μg·kg^(-1) and 0.1 μg·kg^(-1),respectively.The recovery rate of horizontal spiking was 84.9%~88.5%.This method has a high degree of automation and good reproducibility,which can meet the requirements of the determination of aflatoxin B_(1) in grains.