色谱

色谱 ›› 2017, Vol. 35 ›› Issue (4): 427-431.DOI: 10.3724/SP.J.1123.2016.10036

• 研究论文 • 上一篇    下一篇

液相色谱-大气压化学电离串联质谱法测定婴幼儿配方奶粉中的维生素D

严丽娟1, 李文斌2, 洪煜琛1, 吴敏1, 徐敦明1, 林立毅1, 顾春燕2   

  1. 1. 厦门出入境检验检疫局技术中心, 福建 厦门 361026;
    2. 北京迪马科技有限公司, 北京 100029
  • 收稿日期:2016-10-12 出版日期:2017-04-08 发布日期:2013-07-30
  • 通讯作者: 徐敦明,Tel:(0592)7250900,E-mail:xudm@xmciq.gov.cn.
  • 基金资助:

    福建省自然科学基金项目（2016J01071，2014J01057）；长三角科技合作项目（15395810100，16395810100）.

Determination of vitamin D in infant formula using liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry

YAN Lijuan1, LI Wenbin2, HONG Yuchen1, WU Min1, XU Dunming1, LIN Liyi1, GU Chunyan2   

  1. 1. Technology Center of Xiamen Entry-exit Inspection and Quarantine Bureau, Xiamen 361026, China;
    2. Beijing Dikma Technologies Inc., Beijing 100029, China
  • Received:2016-10-12 Online:2017-04-08 Published:2013-07-30
  • Supported by:

    Natural Science Foundation of Fujian Province (Nos. 2016J01071, 2014J01057); Yangtze River Delta Science and Technology Cooperation Project (Nos. 15395810100, 16395810100).

PDF

119

摘要：

建立了婴幼儿配方奶粉中维生素D的液相色谱-大气压化学电离串联质谱（LC-APCI-MS/MS）分析方法。样品经正己烷和甲基叔丁基醚混合溶液提取，ProElut VDC固相萃取柱净化，Kinetex C18色谱柱分离，采用大气压化学电离（APCI）源、正离子扫描和多反应监测（MRM）模式对维生素D2和维生素D3进行检测，内标法定量。结果表明维生素D2和维生素D3在5~5000 μg/L范围内均具有良好的线性关系，检出限为2 μg/kg，定量限为5 μg/kg。在5、10和100 μg/kg添加水平下，维生素D2和维生素D3的回收率为85.2%~105.3%，相对标准偏差为4.7%~8.1%。该方法简便准确，灵敏度高，适用于婴幼儿奶粉中维生素D的测定。

关键词: 维生素D, 液相色谱-大气压化学电离串联质谱, 婴幼儿配方奶粉

Abstract:

A method using liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry (LC-APCI-MS/MS) was developed for the determination of vitamin D in infant formula. The milk powder sample was extracted with hexane and tert-butyl methyl ether followed by clean-up with ProElut VDC cartridge. The LC separation was performed on Kinetex C18 column (100 mm×4.6 mm, 2.6 μm) by a gradient elution using water and acetonitrile as the mobile phases with a flow rate of 1.0 mL/min. Identification of vitamin D2 and vitamin D3 was achieved by APCI-MS/MS using multiple reaction monitoring (MRM). The quantification analysis was performed by internal standard method. The calibration curves showed a good linearity in the range of 5-5000 μg/L. The limits of detection (LODs) for vitamin D2 and vitamin D3 in the formula were 2 μg/kg. The limits of quantification (LOQs) for vitamin D2 and vitamin D3 in the formula were 5 μg/kg. The average recoveries of vitamin D from milk powder spiked at 5, 10 and 100 μg/kg levels were between 85.2% and 105.3%, and the relative standard deviations were between 4.7% and 8.1%. The simple, accurate and sensitive method is suitable for the determination of vitamin D in infant formula.

Key words: infant formula, liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry (LC-APCI-MS/MS), vitamin D

中图分类号: