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采用液相色谱-串联质谱法在线鉴定娃儿藤粗提物中的菲并吲哚里西啶生物碱。

On-line identification of phenanthroindolizidine alkaloids in a crude extract from Tylophora atrofolliculata by liquid chromatography combined with tandem mass spectrometry.

作者信息

Cui Lijie, Abliz Zeper, Xia Min, Zhao Liyan, Gao Song, He Wenyi, Xiang Yun, Liang Feng, Yu Shishan

机构信息

Institute of Materia Medica, Chinese Academy of Medical Sciences and Peking Union Medical College, Beijing 100050, China.

出版信息

Rapid Commun Mass Spectrom. 2004;18(2):184-90. doi: 10.1002/rcm.1297.

DOI:10.1002/rcm.1297
PMID:14745768
Abstract

Electrospray ionization multi-stage tandem mass spectrometry (ESI-MS(n)) and liquid chromatography coupled with sequential mass spectrometry (LC/MS(n)) were applied to identify trace-level phenanthroindolizidine alkaloids in crude extracts from Tylophora atrofolliculata. Based on the relationship between the characteristic fragmentation reactions and the structural features of related compounds of known structure from this plant, the bioactive crude extract was analyzed in detail by positive and negative ion ESI-MS(n), LC/UV-MS and LC/MS(n) techniques. A total of nine constituents in the crude extract were identified rapidly, including several isomers; seven of these constituents are new and two are known compounds. The structures of four of these constituents were subsequently confirmed by nuclear magnetic resonance (NMR) and accurate mass measurements using high-resolution fast-atom bombardment mass spectrometry (FAB-HRMS).

摘要

采用电喷雾电离多级串联质谱法(ESI-MS(n))和液相色谱-串联质谱法(LC/MS(n))对娃儿藤粗提物中的痕量菲并吲哚里西啶生物碱进行鉴定。基于该植物已知结构的相关化合物的特征裂解反应与结构特征之间的关系,采用正、负离子ESI-MS(n)、LC/UV-MS和LC/MS(n)技术对具有生物活性的粗提物进行了详细分析。该粗提物中总共快速鉴定出9种成分,包括几种异构体;其中7种成分为新化合物,2种为已知化合物。随后通过核磁共振(NMR)以及使用高分辨率快原子轰击质谱法(FAB-HRMS)进行精确质量测量,对其中4种成分的结构进行了确认。

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