HO2-钴（III）-博来霉素内部轴向配体的鉴定：博来霉素、去糖博来霉素及其氢过氧化物-钴（III）配合物的1H[15N] HSQC NMR研究

Identification of the internal axial ligand of HO2-cobalt(III)-bleomycin: 1H[15N] HSQC NMR investigation of bleomycin, deglycobleomycin, and their hydroperoxide-cobalt(III) complexes.

作者信息

Xia Chaunwu, Försterling F Holger, Petering David H

机构信息

Department of Chemistry, University of Wisconsin-Milwaukee, P.O. Box 413, Milwaukee, Wisconsin 53201, USA.

出版信息

Biochemistry. 2003 Jun 3;42(21):6559-64. doi: 10.1021/bi030016c.

DOI:10.1021/bi030016c

PMID:12767239

Abstract

The identity of the axial ligand contributed by the drug in hydroperoxide-Co(III)-bleomycin and hydroperoxide-Co(III)-deglycobleomycin has been in doubt. With each structure, a combination of (1)H[(15)N] HSQC and HMBC and (1)H COSY and NOESY NMR spectroscopy was used to observe and completely assign the nonaromatic (15)N chemical shifts of natural abundance bleomycin in the two hydroperoxide-Co(III) structures. Together with the (15)N assignments from a published 1D (15)N spectrum, the results permitted the assignment of the primary amine nitrogen to an axial ligand position in both structures.

摘要

在氢过氧化物 - 钴（III）-博来霉素和氢过氧化物 - 钴（III）-去糖博来霉素中，由药物贡献的轴向配体的身份一直存在疑问。对于每种结构，使用（1）H[(15)N] HSQC和HMBC以及（1）H COSY和NOESY核磁共振光谱的组合，来观察并完全归属天然丰度博来霉素在两种氢过氧化物 - 钴（III）结构中的非芳香族（15）N化学位移。结合已发表的一维（15）N谱的（15）N归属，结果使得在两种结构中都能将伯胺氮归属到轴向配体位置。