Ultra-high resolution band-selective HSQC for nanomole-scale identification of chlorine-substituted 13 C in natural products drug discovery.
Ultra-high resolution band-selective HSQC for nanomole-scale identification of chlorine-substituted 13 C in natural products drug discovery.
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超高分辨率谱带选择性 HSQC，用于天然产物药物发现中氯取代 13 C 的纳摩尔级鉴定。
DOI：
10.1002/mrc.4415
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发表时间：
2017
期刊：
影响因子：
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通讯作者：
Molinski,TadeuszF
中科院分区：
文献类型：
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作者：
Wang,Xiao;Duggan,BrendanM;Molinski,TadeuszF
超高分辨率带选择性HSQC（bsHSQC）已被用于检测35 Cl-37 Cl同位素位移的13 C NMR信号，用于指定溴氯天然产物的区域异构体。探索了最佳脉冲序列和仪器参数，以最大限度地检测同位素位移。氯同位素位移（Δδ）在交叉点内被检测到，并随13 C的杂化、13 C的取代、β-氯取代基的存在以及它们的相对构型而变化。Cl-取代的CH bsHSQC交叉的去卷积可能提供其他有用的信息，包括在卤化天然产物的生物合成过程中定量37 Cl/35 C同位素分馏的潜在MS-独立方法。版权所有© 2016约翰威利父子有限公司.
Ultra‐high resolution band‐selective HSQC (bsHSQC) has been employed for detection of35Cl–37Cl isotope shifted13C NMR signals for assignment of regioisomerism in bromo‐chloro natural products. Optimum pulse sequence and instrumental parameters for maximization of detection of the isotope shifts were explored. The chlorine isotope shifts (Δδ) were detected within crosspeaks and were shown to vary with hybridization of13C, substitution of13C, presence of β‐chloro substituents, and their relative configuration. Deconvolution of Cl‐substituted CH bsHSQC crosspeaks may provide other useful information, including a potentially MS‐independent method for quantitating37Cl/35C isotopic fractionation during the biosynthesis of halogenated natural products. Copyright © 2016 John Wiley & Sons, Ltd.