马钱子发酵物中马钱子碱氮氧化物的NMR数据解析

Analysis of NMR Data of Brucine N-oxide Isolated from Semen Strychni Fermented by Trametes Cinnabarina

目的确定马钱子发酵物所得化合物马钱子碱氮氧化物的结构,对它的1HNMR和13CNMR谱信号进行了归属和详细分析,为其结构鉴定提供了依据。方法从朱红栓菌发酵后的马钱子中提取、分离得到10多种生物碱,其中一种化合物经薄层层析分析,初步认定为马钱子碱氮氧化物。结果以DMSO为溶剂、TMS作内标,采用1HNMR,13CNMR,DEPT,1H-1H COSY,TOCSY,NOESY,HSQC,HMBC等多种核磁共振方法,对它的1H和13C的NMR信号进行了详细分析和精确归属,进一步确定了其结构。结论为马钱子碱氮氧化物的结构鉴定提供了更加可靠的依据。

The ^1HNMR,^13CNMR, distortionless enhancement by polarization transfer （DEFF） and H-^1H correlation spectrometry （COSY）, ^1H-detected heteronuclear single-quantum coherence （HSQC）, nuclear overhauser effect spectroscopy （NOESY）, total correlation spectroscopy （TOCSY）, 1H- detected heteronuclear multiple-bend correlation （HMBC） of brucine N-oxide isolated from Semen strychni fermented by Trametes cinnabarina in DMSO-D6 were obtained and assigned by means of computer simulation of Fourier transform NMR. Detail behaviors of spin - spin splitting of H and its accurate values for the coupling constants are described. The proton and 13carben spectra of the brucine N-oxide were assigned completely. Some mistakes of the proton and 13carbon spectra orientations reported by the former documents are corrected. The experimental results have been shown that the high sensitive DEPT,^1H-^1H COSY, HSQC, NOESY, TOCSY and HMBC are powerful tools to study the microstructure of the similar strychnos alkaloids.