光化学柱后衍生–高效液相色谱法测定婴幼儿营养米粉中的黄曲霉毒素B1

建立婴幼儿营养米粉中黄曲霉毒素B1的高效液相色谱荧光检测器测定方法。样品以甲醇–水(体积比70∶30)溶液匀质提取,过黄曲霉毒素B1免疫层析亲和柱净化,经CNW Athena C18色谱柱分离和光化学柱后衍生反应器衍生后,用带有荧光检测器的高效液相色谱仪测定。采用峰面积外标法定量黄曲霉毒素B1含量。黄曲霉毒素B1在0～10μg/L的浓度范围内线性关系良好,相关系数为0.999 8,检出限为0.25μg/kg。在3个添加水平下加标回收率为97.7%～106.9%,测定结果的相对标准偏差为1.7%(n=6)。该方法的灵敏度、准确度、精密度均符合黄曲霉毒素B1的检测技术要求,适用于婴幼儿营养米粉中黄曲霉毒素B1的日常检测。

Determination of Alfatoxin B1 in Rice Cereal for Infants and Young Children by High Performance Liquid Chromatography Coupled with Post-Column Photochemical Derivatization

A high performance liquid chromatography（HPLC） coupled with post-column photochemical derivatization method was developed for the determination of aflatoxin B1 in rice cereal for infants and young children. The sample was extracted with methanol-water （volume ratio was 70∶30） then purified by immunoaffinity column for the purification aflatoxin B1. The high performance liquid chromatography （HPLC） separation was performed on a CNW Athena C18 column with methanol and water. The aflatoxin B1 was determined by fluorescence detection （FLD） after photochemical derivatization,and quantified by the peak area external standard method. The calibration curve showed good linearity in 0-10 μg/L range with correlation coefficient of 0.999 8. The limit of detection （LOD） was 0.25μg/kg for aflatoxin B1 in rice cereal for infants and young children. The recovery of aflatoxin B1 spiked at there levels in rice cereal for infants and young children ranged from 97.7%to 106.9%with the relative standard deviation（RSD） of 1.7%（n=6）. The sensitivity,accuracy and precision of the method can meet the technical standards requirement of the aflatoxin B1 determination. Therefore the method can be applied to the determination of the aflatoxin B1 in rice cereal for infants and young children.