基于液相高分辨质谱联用与核磁共振技术的甘露特钠结构鉴定  

Structural Identification of Sodium Oligomannate Based on Liquid High Resolution Mass Spectrometry and Nuclear Magnetic Resonance

作　　者：王悦[1] 陈欣桐 刘博[1] 宋玉娟[1] 李俏吟 范慧红[1] WANG Yue;CHEN Xintong;LIU Bo;SONG Yujuan;LI Qiaoyin;FAN Huihong(NMPA Key Laboratory for Quality Research and Evaluation of Chemical Drugs,National Institutes for Food and Drug Control,Beijing 102629,China)

机构地区：[1]中国食品药品检定研究院,国家药品监督管理局化学药品质量研究与评价重点实验室,北京102629

出　　处：《中国药学杂志》2023年第18期1657-1663,共7页Chinese Pharmaceutical Journal

基　　金：青岛海洋科学与技术试点国家实验室海洋药物与生物制品功能实验室开放性课题资助(LMDBKF201806);中国食品药品检定研究院学科带头人培养基金资助(2021X6)。

摘　　要：目的 建立国家一类新药甘露特钠首批国家标准物质,对标准物质的寡糖结构进行确证。方法 采用液质联用、核磁共振等方法确证待标物的结构。液相色谱采用GE Superdex 30 Increase 10/300GL色谱柱对寡糖进行分离,采用负离子模式进行质谱检测;采用一维、二维核磁共振技术,对聚甘露糖醛酸、聚古罗糖醛酸及待标物进行结构分析。结果 通过对质谱、光谱的分析,确证了甘露特钠待标品是以2~10糖组成的寡糖混合物,分子骨架以甘露糖醛酸为主,与理论结构一致。结论 本研究建立了甘露特钠结构确证方法,并对甘露特钠首批对照品的相对分子质量、分子结构进行了确证。OBJECTIVE To establish the first batch of national reference substance(RS)for the first-class new drug sodium oligomannate in China,and confirm the structure of the RS.METHODS Structure of the candidate was confirmed by liquid chromatography-mass spectrometry,nuclear magnetic resonance and other methods.GE Superdex 30 Increase 10/300GL column was used to separate oligosaccharides by liquid chromatography,and negative ion mode for mass spectrometry detection was used;one-dimensional and two-dimensional nuclear magnetic resonance techniques were used to analyze the structures of polymannuronic acid,polyguluronic acid and the sodium oligomannate RS.RESULTS Through the analysis of mass spectrometry and spectrum,it was confirmed that the sodium oligomannate RS is an oligosaccharide mixture composed of 2-10 saccharides,and the molecular backbone is mainly mannuronic acid,which is consistent with the theoretical structure.CONCLUSIONS In this study,the structure confirmation methods of sodium oligomannate are established,and the molecular weight and molecular structure of the first batch of national RS of sodium oligomannate are confirmed.

关 键 词：甘露特钠 高分辨质谱 核磁共振 结构鉴定 国家对照品 甘露糖醛酸 古罗糖醛酸 

分 类 号：R282[医药卫生—中药学]