食品科学

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UPLC-IDMS法测定配方奶粉中的生物素含量

梁敏慧1,崔亚娟2,*,叶 润2,李全霞2,陈兆天2,李菁菁2,李 东2   

  1. 1.北京工业大学生命科学与生物工程学院,北京 100124;2.北京市营养源研究所,北京 100069
  • 出版日期:2015-02-25 发布日期:2015-02-16
  • 通讯作者: 崔亚娟
  • 基金资助:

    北京市科委科技新星计划项目(2011059);卫生部行业科研专项(201202012)

Determination of Biotin in Milk Powder by Using Ultra Performance Liquid Chromatography-Isotope Dilution Mass Spectrometry

LIANG Minhui1, CUI Yajuan2,*, YE Run2, LI Quanxia2, CHEN Zhaotian2, LI Jingjing2, LI Dong2   

  1. 1. College of Life Science and Bioengineering, Beijing University of Technology, Beijing 100124, China;
    2. Beijing Research Institute for Nutritional Resources, Beijing 100069, China
  • Online:2015-02-25 Published:2015-02-16
  • Contact: CUI Yajuan

摘要:

建立一种超高效液相色谱-同位素稀释质谱法测定配方奶粉中生物素含量的方法。样品中加入生物素-D2作为同位素内标,经水超声提取后,以含体积分数0.1%甲酸的10 mmol/L乙酸铵溶液和乙腈作为流动相进行梯度洗脱,采用电喷雾正离子模式、多反应监测方式进行定性定量分析。结果表明:生物素在1~50 ng/mL范围内线性关系良好,线性范围内对已知生物素含量样品3 个标准添加水平的平均回收率为89.6%~93.1%,相对标准偏差为1.71%~4.33%。方法检出限为0.6 μg/100 g,定量限为1.5 μg/100 g,该方法具有灵敏度高、重复性好、分析时间短等优点,可以满足配方奶粉中生物素含量的测定要求。

关键词: 生物素, 超高效液相色谱-同位素稀释质谱, 奶粉

Abstract:

An ultra performance liquid chromatography-isotope dilution mass spectrometry (UPLC-IDMS) method has
been developed for the determination of biotin in milk powder. After spiking biotin-D2 as an internal standard, samples were
extracted with water. The mobile phase consisted of 10 mmol/L ammonium acetate with 0.1% formic acid and acetonitrile.
The biotin was identified under multiple-reaction monitoring (MRM) mode and quantified by an internal standard method.
The results showed a good linear calibration in the range of 1–50 ng/mL, the recoveries at three spiked levels and the relative
standard deviations were 89.6%–93.1% and 1.71%–4.33%, respectively. The limit of detection and quantification for biotin
were 0.6 μg/100 g and 1.5 μg/100 g, respectively. This method is sensitive, time saving, and accurate for the determination
of biotin in milk powder.

Key words: biotin, ultra performance liquid chromatography-isotope dilution mass spectrometry (UPLC-IDMS), milk powder

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