食品科学 ›› 0, Vol. ›› Issue (): 233-235.

• 分析检测 • 上一篇    下一篇

超高效液相色谱质谱联用测定食品中叶酸含量

刘进玺,钟红舰*,董小海   

  1. 农业部农产品质量监督检验测试中心(郑州)
  • 收稿日期:2011-04-22 修回日期:2012-03-12 出版日期:2012-04-25 发布日期:2012-03-31
  • 通讯作者: 刘进玺 E-mail:liujinxi1020@163.com

Determination of Folic Acid in Food by UPLC-MS/MS

  • Received:2011-04-22 Revised:2012-03-12 Online:2012-04-25 Published:2012-03-31

摘要: 建立食品中叶酸含量的超高效液相色谱质谱联用测定方法。样品提取后以Acquity UPLC BEH C18柱(2.1mm×50mm,1.7μm)为色谱柱分离,以电喷雾电离串联质谱在正离子选择反应监测模式下进行测定。以乙腈-0.1%甲酸溶液(5:95,V/V)为流动相、流速0.25mL/min、色谱柱温度40℃、进样量2μL,母离子m/z 442.3、定量子离子m/z 295.1、定性子离子m/z 176.0,碰撞能量为14eV。对空白试样进行3个添加水平4个重复的添加结果表明:回收率80.7%~89.7%,相对标准偏差2.90%~3.85%。该方法检出限1ng/mL,线性范围0.001~1.000μg/mL。该方法具有样品预处理简单、检测周期短、灵敏度较高等优点。

关键词: 叶酸, 测定, 超高效液相色谱/质谱, 食品

Abstract: A method for the determination of folic acid in food by ultra performance liquid chromatography-mass spectrometry/mass spectrometry (UPLC-MS/MS) has been established. Sample extract was separated on Acquity UPLC BEH C18 column (2.1 mm × 50 mm, 1.7 μm) using a mobile phase consisting of acetonitrile and 0.1% formic acid (5:95, V/V) at a flow rate of 0.25 mL/min, and analyzed by electrospray ionization-tandem mass spectrometry (ESI-MS/MS) in a positive-ion selective reaction monitoring (SRM) mode at a collision energy of 14 eV using m/z 442.3, m/z 295.1 and m/z 176.0 as the parent, quantitative and qualitative ions, respectively. The column temperature and the injection volume were set as 40 ℃ and 2 μL, respectively. The average blank spike recoveries for 4 replicate determinations across three spike levels were in the range of 80.7%-89.7% with RSD of 2.90%-3.85%. The limit of detection was 1 ng/mL. An excellent linear relationship was achieved in the range of 0.001-1.000 μg/mL. The method was characterized by simple operation, time saving and high sensitivity.

Key words: folic acid, food, determination, ultra performance liquid chromatography-mass spectrometry/mass spectrometry (UPLC-MS/MS)

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