论文部分内容阅读
建立了免疫亲和柱净化-大体积流通池无需衍生同时测定食品中6种黄曲霉毒素(Aflatoxins)的检测方法。样品采用乙腈-水(84:16,V/V)超声辅助提取,用免疫亲和柱净化,经过XBridge TM C18柱(150 mm×4.6 mm,5μm)分离。采用乙腈-甲醇-水(15:25:60,V/V)为流动相,大体积流通池荧光检测器检测,无需衍生,外标法定量。6种黄曲霉毒素在9.5 min内有效分离,从样品前处理到结果分析整个过程小于50 min。黄曲霉毒素B1、B2、G1、G2、M1、M2的检出限(LOD,S/N=3)分别为0.05μg/kg、0.02μg/kg、0.05μg/kg、0.02μg/kg、0.04μg/kg、0.03μg/kg,能够满足我国对食品中黄曲霉毒素限量的要求。6种黄曲霉毒素标准曲线线性良好,线性相关系数r2大于0.999;样品加标回收率为77.6%~90.5%,精密度RSD为2.42%~6.08%。本方法简便、准确、灵敏度高,无需衍生即可同时检测食品中6种黄曲霉毒素,适用于食品中6种黄曲霉毒素的快速定量测定。
An immunoaffinity column purification system was developed for the detection of six aflatoxins in foodstuff without the need of derivatization in a large volumetric flow cell. Samples were sonicated with acetonitrile-water (84:16, V / V) and purified by immunoaffinity column and separated on a XBridge ™ C18 column (150 mm × 4.6 mm, 5 μm). Acetonitrile-methanol-water (15:25:60, V / V) was used as the mobile phase. Large-volume flow cytometry fluorescence detector was used for detection without derivatization and external standard method. Six aflatoxins were efficiently separated within 9.5 min, from sample preparation to analysis of results for less than 50 min. The detection limits (LOD, S / N = 3) of aflatoxins B1, B2, G1, G2, M1 and M2 were 0.05μg / kg, 0.02μg / kg, μg / kg, 0.03μg / kg, to meet our country aflatoxin food requirements. The standard curve of six aflatoxins showed good linearity and the linear correlation coefficient r2 was greater than 0.999. The spiked recoveries were 77.6% -90.5% and the RSDs were 2.42% -6.08%. The method is simple, accurate and sensitive, and can simultaneously detect six kinds of aflatoxins in foods without being derived, and is suitable for the rapid and quantitative determination of six aflatoxins in foods.