磁性多壁碳纳米管固相萃取-液质联用法测定植物油中的黄曲霉毒素B1

Determination of Aflatoxin in Vegetable Oils by Liquid Chromatography-mass Spectrometry with Magnetic Multi-walled Carbon Nanotubes Solid Phase Extraction

以化学共沉淀法制备的MWCNTs-Fe3O4为磁性吸附剂,结合高效液相色谱串联质谱测定植物油中的黄曲霉毒素。样品加入正己烷后,用pH=3.0、体积分数为12.5%的乙腈—水溶液提取,最后加入MWCNTs-Fe3O4进行磁性固相萃取。优化了萃取剂、吸附剂用量、吸附时间、洗脱剂、洗脱时间等磁性固相萃取条件。结果表明,黄曲霉毒素AFB1其线性范围内线性关系良好,相关系数为0.9987,方法检出限为0.01μg/kg,定量限为0.04μg/kg。在样品中分别添加水平为5,10和20μg/kg的AFB1,回收率为81.5%~104.5%,相对标准偏差为1.5%~4.3%。该方法简便、快速、准确,可用于植物油中黄曲霉毒素AFB1的检测。

Aflatoxins in vegetable oil were determined by HPLC tandem mass spectrometry with MWCNTs-Fe3O4 which prepared by chemical co-precipitation as magnetic adsorbent. After adding n-hexane,the samples were extracted by acetonitrile-water solution with a pH of 3.0 and a volume fraction of 12.5%,and purified by MWCNTs-Fe3O4. The magnetic solid phase extraction conditions such as extraction agent,adsorbent dosage,adsorption time,eluent and eluent time were optimized. The results showed that aflatoxin AFB1 had a good linearity with the correlation coefficient of 0.9987. The LOD was 0.01μg/kg and the LOQ was 0.04μg/kg. The average recoveries at spiked levels of 5,10,20 μg/kg ranged from 81.5% to104.5% with relative standard deviations between 1.5% and 4.3%. The method is simple,rapid and accurate for the determination of AFB1 in vegetable oil.