高效液相色谱-电喷雾多级质谱法对格尔德霉素粗品中各组分的初步判别及分类  

Preliminary discrimination and assortment of the components in the crude geldanamycin preparation by HPLC-ESI-MS^n

作　　者：朱健 周璟明[2] 陈晓霞 谢颖[2] 陈秀明[2] 方东升[2] 郑卫[2] 

机构地区：[1]杭州华东医药集团生物工程研究所有限公司,杭州310011 [2]福建省微生物研究所福建省新药(微生物)筛选重点实验室,福州350007

出　　处：《中国抗生素杂志》2011年第3期207-213,共7页Chinese Journal of Antibiotics

摘　　要：目的对格尔德霉素(GDM)粗品中各组分进行与质量数相关的结构信息方面的初步判别及分类。方法应用高效液相色谱-电喷雾多级质谱法(LC-ESI-MSn)在正离子模式下对粗品进行分析。结果通过与对照品的液质比对,确定GDM粗品中MW=560.3(25.0min)、MW=1024.7(36.8min)分别为GDM、洋橄榄素,并首次研究了洋橄榄素的正离子模式质谱裂解规律。通过对GDM粗品中各组分多级质谱碎片信息的分析整理,结合已知物的裂解规律,归纳发现GDM粗品中主要含有三大类物质:以GDM为主成分的含有氨甲酰基的苯安莎类物质(10~35min)、洋橄榄素及其同系物(35~50min)、一组分子量相差74u的未知物(50~65min)。结论 LC-ESI-MSn能快速地对GDM粗品中各组分进行初步的结构分析,通过本实验建立了一套利用LC-ESI-MSn对复杂样品中化合物的快速结构归属的方法,为微生物新药的快速结构筛选研究提供一定参考作用。Objective To analyze the components existed in the crude geldanamycin （GDM） preparation. Methods The crude GDM product was analyzed by HPLC-ESI-MSn under the positive mode. Results Compared with the reference substance by LC-MSn, the compounds eluted at 25.0min and 36.8min were identified as GDM and elaiophylin, respectively. The fragmentation pathways of elaiophylin in MS under positive mode were reported for the first time. Based on the ESI-MSn（＋） spectra of these components in the crude extract, and the known fragmentation pathways of GDM and elaiophylin, the components in crude GDM product could be classified into three main kinds of compounds as follows： a series of benzoquinoid ansamycins with geldanamycin as the main product （10-35min）; elaiophylin and its homologues （35-50min）; a series of unknown polymers with 74u difference in molecular weight （50-65min）. Conclusion Preliminary analysis of the structures of components in the crude GDM preparation can be done successfully by LC-MS method which is useful in rapid screening for novel microbial products.

关 键 词：电喷雾多级质谱 格尔德霉素 洋橄榄素 质谱裂解规律 

分 类 号：TQ460[化学工程—制药化工]