基于多巴胺-氧化石墨烯复合物的搅拌棒吸附萃取/高效液相色谱法测定食用油中黄曲霉毒素

Determination of Aflatoxins in Edible Oil by High Performance Liquid Chromatography with Stirring Bar Sorptive Extraction Based on Dopamine-Graphene Oxide Complex

建立了一种基于贻贝仿生化学涂层的搅拌棒吸附萃取/高效液相色谱/荧光检测器(SBSE/HPLC-FLD)同时测定食用油中黄曲霉毒素B1、B2、G1、G2的方法。基于贻贝仿生化学制备多巴胺-氧化石墨烯复合物固相萃取材料,利用搅拌棒吸附萃取技术对样品进行提取;以甲醇-乙腈-水(10%磷酸调至p H 3.5,体积比3∶3∶5)作为流动相,采用荧光检测器进行检测。结果显示,黄曲霉毒素B1、B2、G1、G2在0.200~10.0μg/L范围内具有良好的线性关系(相关系数r^2≥0.998 9),加标回收率为81.5%~96.9%,日内相对标准偏差(RSD)为1.7%~3.4%,日间RSD为1.9%~3.5%,方法检出限为0.025~0.050μg/L。该方法高效、灵敏、可靠,能够满足食用油中黄曲霉毒素B1、B2、G1、G2的测定要求。

A method of stirring bar sorptive extraction(SBSE)based on mussel-bioinspired chemistry coating and high performance liquid chromatography with fluorescence detector(HPLC/FLD)was developed for the simultaneous determination of aflatoxin B1,B2,G1 and G2(AFB1,AFB2,AFG1 and AFG2)in edible oil.The sample was extracted by SBSE with dopamine-graphene oxide complex as solid phase extraction material prepared by mussel-bioinspired chemistry.The target compounds were separated on a Kromasil C 18 column using methanol-acetonitrile-water aqueous solution(3∶3∶5 by volume,adjust pH 3.5 with 10%phosphoric acid)as mobile phases,and detected with a fluorescence detector.The calibration curves for AFB1,AFB2,AFG1 and AFG2 were linear in the concentration range of 0.200-10.0μg/L,with their correlation coefficients(r 2)not less than 0.998 9.The spkied recoveries for 4 aflatoxins(AFs)in edible oil samples ranged from 81.5%to 96.9%,with intra-day relative standard deviations(RSDs)of 1.7%-3.4%and inter-day RSDs of 1.9%-3.5%.The limits of detection(LODs)were in the range of 0.025-0.050μg/L.The proposed method is efficient,sensitive and reliable,and is suitable for the determination of AFB1,AFB2,AFG1 and AFG2 in edible oil.