高效液相色谱-串联质谱法快速检测粮油制品中黄曲霉毒素B1的含量

Rapid determination of aflatoxin B1 in grain and oil products by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  液相色谱-串联质谱法  粮油制品  黄曲霉毒素B1

英文关键词:liquid chromatography-mass spectrometry  grain and oil products  aflatoxin B1

中文摘要:

      目的 建立高效液相色谱-串联质谱法快速测定粮油制品中黄曲霉毒素B1含量的分析方法。方法 样品中的黄曲霉毒素B1经提取、免疫亲和柱净化、浓缩等步骤, 以5 mmol/L乙酸铵溶液、乙腈-甲醇溶液(50:50, V:V)为流动相, 按照梯度洗脱程序, 通过液相色谱-串联质谱法进行测定, 外标法定量。结果 黄曲霉毒素B1在0.2~20 ng/mL浓度范围内与峰面积呈现良好的线性关系, 线性方程为Y=68577.3X?20845, r>0.998, 加标回收率在85.0%~94.1%之间, 相对标准偏差(relative standard deviation, RSD)<5.5%, 方法检出限和定量限分别为0.07和0.2 μg/kg。结论 该方法测定结果准确、可靠, 可用于快速测定粮油制品中黄曲霉毒素B1的含量。

英文摘要:

      Objective To establish a rapid method for the determination of aflatoxin B1 in grain and oil products by high performance liquid chromatography-tandem mass spectrometry. Methods Samples were extracted, purified and concentrated by immunoaffinity column. Using 5 mmol/L ammonium acetate solution and acetonitrile-methanol solution (50:50, V:V) as mobile phase, according to gradient elution procedure, the samples were determined by liquid chromatography-tandem mass spectrometry and quantified by external standard method. Results There was a good linear relationship between aflatoxin B1 concentration and peak area in the range of 0.2?20 ng/mL, the linear equation was Y=68577.3X?20845, r> 0.998. The recoveries of aflatoxin B1 were 85.0%?93.3% and RSDs were less than 5.5%, the limit of detection and limit of quantitative were 0.07 and 0.2 μg/kg, respectively. Conclusion This method is accurate and reliable, which can be used for the rapid determination of aflatoxin B1 in grain and oil products.