郝庆秀;康利平;朱寿东;余意;胡明华;马方励;周洁;郭兰萍;
HAO Qing-xiu;KANG Li-ping;ZHU Shou-dong;YU Yi;HU Ming-hua;MA Fang-li;ZHOU Jie;GUO Lan-ping;The State Key Laboratory Breeding Base of Dao-di Herbs,National Resource Center for Chinese Materia Medica,China Academy of Chinese Medical Sciences;Infinitus ( China) Company Ltd.;University of Ji'nan;

• 1:中国中医科学院中药资源中心道地药材国家重点实验室培育基地
• 2:无限极(中国)有限公司
• 3:济南大学

摘要(Abstract)：

建立了巴戟天低聚糖成分快速鉴定的超高效液相色谱串联四级杆飞行时间质谱(UPLC-Q-TOF-MS~E)的方法。利用UPLC-Q-TOF-MS~E,对巴戟天低聚糖成分进行在线快速分析鉴定。以水-乙腈为流动相,梯度洗脱,ESI正、负离子模式下采集数据,通过UNIFI数据库检索并人工复核相对分子质量、特征离子、中性丢失、以及色谱保留行为等信息,并结合对照品信息和文献信息对其进行验证;对于未知成分,根据其精确相对分子质量、质谱裂解碎片、色谱保留时间、以及已知同类化合物的碎片特征,对其进行结构推测。该实验鉴定了19个巴戟天低聚糖成分,为巴戟天药材的创新性开发利用研究提供了科学依据。
In this paper,an approach was applied for separation and identification of oligosaccharides in Morinda officinalis How by Ultra performance liquid chromatography/quadrupole time-of-flight mass spectrometry( UPLC-Q-TOF-MS) with collision energy. The separation was carried out on an ACQUITY UPLC BEH Amide C_(18)( 2. 1 mm × 100 mm,1. 7 μm) with gradient elution using acetonitrile( A) and water( B) containing 0. 1% ammonia as mobile phase at a flow rate of 0. 2 m L·min~(-1). The column temperature was maintained at 40 ℃. The information of accurate mass and characteristic fragment ion were acquired by MS~Ein ESI negative mode in low and high collision energy. The chemical structures and formula of oligosaccharides were obtained and identified by the software of UNIFI and Masslynx 4. 1 based on the accurate mass,fragment ions,neutral losses,mass error,reference substance,isotope information,the intensity of fragments,and retention time. A total of 19 inulin oligosaccharide structures were identified including D( +)-sucrose,1-kestose,nystose,1 F-fructofuranosyl nystose and other inulin oligosaccharides( DP 5-18). This research provided important information about the inulin oligosaccharides in M. officinalis. The results would provide scientific basis for innovative utilization of M. officinalis.

关键词(KeyWords)： 巴戟天;低聚糖;鉴别;UPLC-Q-TOF-MS~E;UNIFI数据库
Morinda officinalis;oligosaccharide;identification;UPLC-Q-TOF-MS~E;UNIFI

Abstract:

Keywords:

基金项目(Foundation): 中国中医科学院基本科研业务费自主选题项目;中国中医科学院重点领域项目(ZZ/0-027);; 国家重点研发计划项目(2017YFC1700701);; 北京中医药薪火传承3+3工程项目

作者(Author): 郝庆秀;康利平;朱寿东;余意;胡明华;马方励;周洁;郭兰萍;
HAO Qing-xiu;KANG Li-ping;ZHU Shou-dong;YU Yi;HU Ming-hua;MA Fang-li;ZHOU Jie;GUO Lan-ping;The State Key Laboratory Breeding Base of Dao-di Herbs,National Resource Center for Chinese Materia Medica,China Academy of Chinese Medical Sciences;Infinitus ( China) Company Ltd.;University of Ji'nan;

Email:

DOI: 10.19540/j.cnki.cjcmm.2018.0046

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