液相色谱-串联质谱法测定食用油中4种黄曲霉素

Determination of Four Aflatoxins in Edible Oil by Liquid Chromatography-tandem Mass Spectrometry

建立了液相色谱-串联质谱法(LC-MS/MS)同时测定食用油中4种黄曲霉素的方法。样品用正己烷溶解,55%甲醇水溶液提取,用三氯甲烷反萃取,流动相定容。C8色谱柱分离,在电喷雾正离子模式下电离,并采用多反应监测(MRM)采集数据方式定性定量分析。4种黄曲霉素在0.75~20μg/kg浓度范围内线性良好,相关系数均大于0.999;在三个不同浓度添加水平下,平均回收率为83.0%~95.0%,相对标准偏差(RSD)为7.5%~13.1%;检出限(LOD)为0.15~0.2μg/kg;定量限(LOQ)为0.75~0.8μg/kg。该方法简便快速、灵敏可靠,适用于食用油中四种黄曲霉素的同时快速测定。

The method for the determination of four aflatoxins （B1, B2, Gh G2, M1） in edible oil by liquid chromatography-tandem mass spectrometry was developed. The sample was dissolved with n-hexane, then extracted with 55 % （V/V） methanol water solution, followed by counter extracted by trichloromethane and diluted with mobile phase.The tour aflatoxins were separated on a C8 column followed by positive electrospray ionization and multi-reaction monitoring（MRM） provided by triple-quadrupole tandem mass spectrometer. Good linearity can be obtained in the concentration range of 0.75-20p.g/kg with the correlation coefficients higher than 0.999. The spiked recoveries were within 83.0 %-95.0 % at the three spiked levels for all the four aflatoxins with the relative standard deviations （RSDs） 0.15-0.2μg/kg. The detection limits （LOD） of the four aflatoxins were 0.75-0.8μg/kg. The developed method is sensitive, accurate and reliable, and it can be applied to the determination of the four aflatoxins in edible oil.