食品科学 ›› 2019, Vol. 40 ›› Issue (16): 321-326.doi: 10.7506/spkx1002-6630-20180920-223

• 安全检测 • 上一篇    下一篇

高效液相色谱-电感耦合等离子体质谱法测定配方食品中的VB12

刘 杰,龚 蕾,朱晓玲,彭青枝,张 莉,周陶鸿,江 丰,黄 茜,张小玲   

  1. 湖北省食品质量安全监督检验研究院,湖北省食品质量安全检测工程技术研究中心,湖北 武汉 430070
  • 出版日期:2019-08-25 发布日期:2019-08-26
  • 基金资助:
    湖北省食品质量安全监督检验研究院自主立项项目(ZZLX2015007)

Determination of VB12 in Formula Foods by High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

LIU Jie, GONG Lei, ZHU Xiaoling, PENG Qingzhi, ZHANG Li, ZHOU Taohong, JIANG Feng, HUANG Qian, ZHANG Xiaoling   

  1. Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test, Hubei Provincial Institute for Food Supervision and Test, Wuhan 430070, China
  • Online:2019-08-25 Published:2019-08-26

摘要: 建立高效液相色谱-电感耦合等离子体质谱测定配方食品中VB12的方法。样品经预处理后采用HLB固相萃取小柱净化,C18反相色谱柱(100 mm×2.1 mm,3 μm)进行分离,甲醇-8 mmol/L乙酸铵溶液(19∶81,V/V)为流动相,等度洗脱,用电感耦合等离子体质谱测定钴离子浓度并间接测定样品中VB12的含量。结果表明,在7 min内可完成化合物的分析,目标化合物峰形较好,VB12在0.1~500 μg/L范围内线性关系良好,相关系数为0.999,检出限为0.02 μg/kg,不同食品基质在高、中、低3 个添加水平下的平均回收率在81.3%~103.6%之间,相对标准偏差在0.4%~4.6%之间。本方法简便、快速、灵敏度高、抗基质干扰能力强、动态范围宽,可用于各类配方食品中VB12的测定。

关键词: 高效液相色谱-电感耦合等离子体质谱, 配方食品, VB12

Abstract: A method based on high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS) was developed for determination of VB12 in formula foods. The sample pretreatment was performed followed by purification using an HLB solid phase extraction column, and then the analyte was separated on a C18 reversed phase column by isocratic elution using a mobile phase consisting of methanol and 8 mmol/L ammonium acetate aqueous solution (19:81, V/V). VB12 was determined indirectly by measuring cobalt ions in samples by ICP-MS. The results showed that the analysis could be completed within 7 min, and the target compound exhibited a good peak shape. A good linearity was obtained in the range of 0.1–500 μg/L for VB12 with a correlation coefficient of 0.999. The limit of detection (LOD) was 0.02 μg/kg. The average recoveries of the method ranged from 81.3% to 103.6% with relative standard deviations of 0.4% to 4.6% for different food matrixes at three spiked levels (n = 6). The method is simple, fast and sensitive with strong resistance to matrix interference and wide dynamic range. It is applicable to various formula foods.

Key words: high performance liquid chromatography-inductively coupled plasma-mass spectrometry, formula food, VB12

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