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机构地区:[1]河南出入境检验检疫局,郑州450003 [2]郑州大学化学系,郑州450042
出 处:《理化检验(化学分册)》2013年第8期981-984,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基 金:河南省科技攻关项目(122102310456);国家质检总局科研计划项目(2007IK162)资助
摘 要:提出了高效液相色谱法测定花生油、橄榄油和芝麻油等3种植物油中4种黄曲霉毒素B,、Bz、G·和Gz的含量。样品采用55%(体积分数)甲醇溶液提取后,经免疫亲和柱净化,流出液中的黄曲霉毒素在YMCODS-AQS-3色谱柱上用含溴化钾120mg和硝酸350μL的甲醇-乙腈~水(25+17+60)混合液作流动相进行色谱分离,并经衍生化后进行荧光检测,所用激发及发射波长依次为362,440nm。4种黄曲霉素的质量浓度分别在一定范围内与其对应的峰面积呈线性关系,黄曲霉毒素B1、G1、B2和G2的测定下限(10S/N)依次为0.4,0.4,0.2,0.2肚g·kg。在3个浓度水平下进行加标回收试验,方法的回收率在74%~112%之间,测定值的相对标准偏差(n=10)在3.6%~15%之间。HPLC with fluorescence detector was applied to the determination of 4 aflatoxins (i. e. , AF B1, AF Be, AF G and AF G2 ) in 3 vegetable oils (i. e. , peanut oil, olive oil and sesame oil). The sample was extracted with 55 (p) methanol solution and purified by IAC. Aflatoxins in the eluate were separated on MC ODS AQ S-3 column with a mixture of CHaOH-CH3CN-H20(25+17+60) containing 120 mg of KBr and 350 μL of HNO: as mobile phase. After derivatization, fluorescence detections with Ae, of 362 nm and ;e,1 of 440 nm were adopted in the determination. Linear relationships between values of peak area and mass concentration of the 4 aflatoxins were obtained in the definite ranges, with lower limits of determination (10S/N) of 0. 4 /,g kg 1 for B1 and G, and 0. 2μg kg -1 for Be and G2. Tests for recovery were performed by standard addition method at 3 concentration levels, giving values of recovery and RSD's (n=10) in the range of 74/00-112/00 and 3.6%--15% respectively.
关 键 词:黄曲霉毒素 高效液相色谱荧光检测法 植物油
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