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

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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).

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

CLC Number: