高效液相色谱-串联质谱法测定山茶油中黄曲霉毒素B1

建立了山茶油中黄曲霉毒素B1含量的高效液相色谱-串联质谱分析方法。通过对前处理方法的优化,选择了甲醇和水作为山茶油中黄曲霉毒素B1的提取溶剂,经免疫亲和柱富集浓缩后,采用高效液相色谱-串联质谱进行分析,经C18色谱柱分离,在电喷雾离子化正离子模式(ESI+)及多反应监测模式(MRM)下进行测定,基质匹配标准溶液外标法定量。在优化条件下,该方法线性范围为0.4～6.4μg/L,相关系数r2>0.998,最低检出限为0.026μg/kg,在添加水平为0.008,0.016和0.032μg时,方法回收率在85.9%～93.8%之间;相对标准偏差为1.8%～5.0%。方法可满足山茶油中黄曲霉毒素B1的检测要求。

Determination of aflatoxin B1 in camellia seed oil by liquid chromatography-tandem mass spectrometry

In order to improve detection sensitivity and accuracy of aflatoxions,a liquid chromatography-tandem mass spectrometric method was established for qualitative and quantitative analysis of aflatoxins B1.Samples were simply extracted by methanol-water at a ratio of 70:30(V/V).After being filtered,it was cleaned up with an immunoaffinity column.The analysis was realized by multiple reaction-monitoring mode.Under above conditions,aflatoxins B1 could be completely separated within 10 min with an excellent linear relationship.The determination limit for aflatoxin B1 was 0.012 μg/kg.The recoveries of samples were in the range of 85.9 %-93.8 % with a relative standard deviation less than 5%.This method can provide a rapid,sensitive,accurate and reproducible detection for aflatoxin B1 and its detection limit is sensitive enough to meet the European regulation for aflatoxins.