摘要
对海南半红树植物黄槿(Hibiscus tiliaceus)内生菌中提取的一个新化合物进行核磁共振结构解析的研究.在核磁共振测试时发现水峰信号与部分样品信号发生了重叠,直接影响了该化合物谱图数据的分析.本工作通过实验确证了在氘代二甲亚砜(DMSO-d6)溶剂中水峰化学位移与含水量之间的变化规律.依据该规律,利用定量加入纯水的方法对实际样品中的水峰信号进行了调制,解决了水峰信号与样品信号的重叠问题,得到了较理想的1HNMR,13CNMR一维谱和COSY,HMQC,HMBC等二维谱.利用核磁共振提供的信息完成了对新化合物结构的解析,确定该化合物为齐墩果烷三萜类化合物3,4-seco-olean-11,13-dien-4,15α,22β,24-tetraol-3-oic acid.
The structure of a new compound, isolated from the endophyte of the semi-mangrove plant Hibiscus tilianceus, was elucidated with nuclear magnetic resonance spectroscopy. In the primary ^1H NMR test, it was found that some signal lines were submerged under the ＂water peak＂, and this would interfere with the analysis of NMR spectra. In this work, the variational rule between the water-peak chemical shift and the water content was investigated for solvent DMSO-d6. Using the results, the water-peak chemical shift was modulated with certain amount of extra water introduced into the practical sample tests. As a resuit, the interference of water peak was overcome, and a group of suitable spectra including ^1HNMR, ^13CNMR, COSY, HMQC, HMBC, etc., were obtained. The structural elucidation of the new compound was achieved, and it was confirmed that this compound belonged to a triterpenoid of oleanane, and identified as 3,4-seco-olean-11,13-dien-4,15a,22β,24-tetraol-3-oic acid.
出处
《化学学报》
SCIE
CAS
CSCD
北大核心
2008年第11期1327-1332,共6页
Acta Chimica Sinica
关键词
核磁共振(NMR)
水峰调制
结构解析
齐墩果烷型三萜
nuclear magnetic resonance （NMR）
modulation of water peak
structural elucidation
triterpenoid of oleanane
