HPLC Determination of 4 Aflatoxins in 3 Vegetable Oils
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B1、B2、G1和G2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YMC ODS-AQ S-3色谱柱上用含溴化钾120 mg和硝酸350 μL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362,440 nm。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 μg·kg-1。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。
Abstract
HPLC with fluorescence detector was applied to the determination of 4 aflatoxins (i.e., AF B1, AF B2, AF G1 and AF G2) in 3 vegetable oils (i.e., peanut oil, olive oil and sesame oil). The sample was extracted with 55% (φ%) methanol solution and purified by IAC. Aflatoxins in the eluate were separated on YMC ODS-AQ S-3 column with a mixture of CH3OH-CH3CN-H2O(25+17+60) containing 120 mg of KBr and 350 μL of HNO3 as mobile phase. After derivatization, fluorescence detections with λex of 362 nm and λem 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 μg·kg-1 for B1 and G1, and 0.2 μg·kg-1 for B2 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%-112% and 3.6%-15%, respectively.
中图分类号 O652.63
所属栏目 工作简报
基金项目 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
收稿日期 2012/6/11
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备注祝伟霞(1979-),女,河南太康人,工程师,硕士,主要从事食品安全检测技术研究。
引用该论文: ZHU Wei-xia,YANG Ji-zhou,YUAN Ping,WANG Cai-juan,WEI Wei. HPLC Determination of 4 Aflatoxins in 3 Vegetable Oils[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2013, 49(8): 981~984
祝伟霞,杨冀州,袁萍,王彩娟,魏蔚. 高效液相色谱法测定3种植物油中4种黄曲霉毒素含量[J]. 理化检验-化学分册, 2013, 49(8): 981~984
被引情况:
【1】谢昕,李红艳, "免疫亲和柱净化-光化学柱后衍生-高效液相色谱法测定柏子仁中的黄曲霉毒素",理化检验-化学分册 52, 541-544(2016)
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参考文献
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【10】TANAKA H, TAKINO M, SUGITA-KONISHI Y, et al. Development of a liquid chromatography/time-of-flight mass spectrometric method for the simultaneous determination of trichothecenes, zearalenone and aflatoxins in food stuffs[J]. Rapid Communi Mass Spectro, 2006,20(9):1422-1428.
【2】LI Pei-wu, ZHANG Qi, ZHANG Wen. Immunoassays for aflatoxins[J]. Trends in Anal Chem, 2009,28(9):1115-1126.
【3】GB 2761-2011食品安全国家标准 食品中真菌毒素限量[S].
【4】LI Pei-wu, ZHANG Qi, ZHANG Wen, et al. Development of a classspecific monoclonal antibody based ELISA for aflatoxins in peanut[J]. Food Chem, 2009,115(1):313-317.
【5】GB 5009. 24-2010 食品安全国家标准 食品中黄曲霉毒素M1和B1的测定[S].
【6】BAO L, TRUCKSESS M W. Determination of aflatoxins B1, B2, G1 and G2 in olive oil, peanut oil and sesame oil[J]. J AOAC Int, 2010,93(3):936-942.
【7】IDRIS Y M A, MARIOD A A, ELNOUR I A, et al. Determination of aflatoxin levels in Sudanese edible oils[J]. Food Chem Toxic, 2010,48(8/9):2539-2541.
【8】NONAKA Y, SAITO K, HANIOKA N, et al. Determination of aflatoxins in food samples by automated on-line in-tube solid-phase microextraction coupled with liquid chromatography-mass spectrometry[J]. J Chromatogra A, 2009,1216(20):4416-4422.
【9】CAVALIERE C, FOGLIA P, GUARINO C, et al. Determination of aflatoxins in olive oil by liquid chromatography-tandem mass spectrometry[J]. Ana Chim Acta, 2007,596(1):141-148.
【10】TANAKA H, TAKINO M, SUGITA-KONISHI Y, et al. Development of a liquid chromatography/time-of-flight mass spectrometric method for the simultaneous determination of trichothecenes, zearalenone and aflatoxins in food stuffs[J]. Rapid Communi Mass Spectro, 2006,20(9):1422-1428.
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