Chinese Journal of Chromatography

Chinese Journal of Chromatography

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Preparation of 1-(2-naphthyl)-3-methyl-5-pyrazolone as pre-column derivatization reagent for the determination of saccharides using high performance liquid chromatography-mass spectrometry

SUN Zhiwei1, LIU Lingjun1, HU Baojun1, SHENG Xiao1, WANG Xiaoyan2, SUO Yourui2, YOU Jinmao1,2   

  1. 1.Key Laboratory of Life-Organic Analysis of Sandong Province, College of Chemistry Science, Qufu Normal University, Qufu 273165, China; 2.Northwest Plateau Institute of Biology, the Chinese Academy of Sciences, Xining 810001, China
  • Received:2007-09-11 Revised:2007-12-10 Online:2008-03-30 Published:1984-06-25

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Abstract:

Eight saccharides were derivatized using 1-(2-naphthyl)-3-methyl-5-pyrazolone (NMP) as pre-column derivatizing reagent， and separated on a reversed-phase Hypersil ODS 2 column (4.6 mm×200 mm, 5 μm), by high performance liquid chromatography (HPLC) in conjunction with a gradient elution, detected by a diode array detector (DAD), and identified by electrospray ionization-mass spectrometry (ESI-MS) in positive ion mode. NMP reacted with reductive saccharides easily in the presence of 17% ammonia water at 70 ℃. All linear correlation coefficients for saccharide derivatives were over 0.9985. The detection limits （at signal-to-noise of 3∶1） were 0.58-1.1 pmol for saccharide derivatives. The characteristic fragment ions, especially m/z 473, from the cleavage of NMP-labeled saccharides exhibited high regularity for the identification of the composition of saccharide mixture. The established method is sensitive and repeatable for the determination of saccharides.

Key words: 1-(2-naphthyl)-3-methyl-5-pyrazolone, saccharides , high performance liquid chromatography-mass spectrometry (HPLC-MS): pre-column derivatization