MS/MS技术在确定清香桂碱A和A_1混晶结构中的应用

APPLICATION OF FAB-MS / MS TECHNIQUE IN STRUCTURAL DETERMINATION OF SARCORUCININE A AND A_1

清香桂(Sarcococca ruscifolia)植物中得到一个清香桂碱A和A_1的共晶,我们通过化学及光谱方法确定了清香桂碱A_1及B的化学结构,并用MS/MS技术证实了这个混晶的结构。这几个生物碱的结构为,碱A(1)为Δ^(14,16)-3α-二甲胺孕甾二烯;碱A_1(2)为Δ^(16)-3α-甲基甲酰胺孕甾烯;碱B(5)为Δ^(16)-3α-二甲胺孕甾烯-20-酮。

From Sarcococca ruscifolia, the mixed crystal of sarcorucinine A and A, were obtained, but was very difficulty in separating. The structure of sarcorucinine A was determined by X-ray analysis for the mixed crystal. Compounds 3 and 4 were isolated from the reduction of mixed crystal with LiAlH4, and their structures were elucidated on the basis of the interpretation of MS, IR, 1H, and 13C NMR spectra. Thus, the structrue of sarcorucinine A, could be deduced as △163α-dimethylamino-20α-methylmethylamido-pregnene (2), and was further comfired by FAB-MS / MS spectra. The structure of the sarcorucinine B was deduced by using the same spectroscopic analysis. The present paper deals with the application of FAB-MS / MS technique in structural elucidation of sarcorucinine A, A, and structural elucidation of sarcorucinine B.