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目的对中药半夏中在C18色谱柱上保留较弱的化学成分进行分离与鉴定。方法首先采用Waters X-Bridge C18色谱柱(150mm×4.6mm,5μm)对半夏药材酸水提取液进行分离,然后对半夏提取液中在C18柱上保留较弱的成分采用Tech Mate TX色谱柱(120A,150mm×2.0mm,5μm)(SCX与反相C18混合填料色谱柱)进行进一步分离分析,最后采用LC-MS对所分离成分进行鉴定,ESI正离子模式扫描分析。结果根据正离子模式下获得的各色谱峰的质谱数据,共检测到13个主要的化学成分,其中3个通过与文献对照或根据质谱裂解规律得到了确认,分别为:缬氨酸,腺嘌呤,精氨酸;化合物1,2,4,5,7,8和13推测为:5-羟甲基糠醛,6 H-purin-6-1,2-amino-1,9-dihydro-8-(1-naphthalenylamino),环-(缬氨酸-酪氨酸),环-(亮氨酸-酪氨酸),亮氨酸-异亮氨酸,(-)-pohakulin pohakuline,N-(1-(苯基乙酰基)-L-脯氨酰)甘氨酸乙酯,化合物9推测为某种环肽;化合物10和11由于缺乏相关对照品和相关文献报道,其结构有待进一步分析鉴定。结论在C18柱上死时间内流出而不能很好分离的物质,在混合填料柱上得到了进一步分离,这说明在某种程度上,采用单一固定相不能很好分离的某些化合物可以采用混合固定相色谱柱达到进一步分离,尤其是在对复杂体系样品的分离及鉴定过程中,混合固定相色谱柱将具有良好的应用前景。
OBJECTIVE To isolate and identify the weak chemical constituents of Cynanchum Phellodendri on C18 column. Methods The Waters X-Bridge C18 column (150mm × 4.6mm, 5μm) was used to separate the aqueous acid extracts of Pinellia ternata, and then the weaker components of the Pinellia ternata extract on C18 column were separated by Tech Mate TX chromatography Column (120A, 150mm × 2.0mm, 5μm) (SCX and reversed-phase C18 mixed packed column) for further separation and analysis, and finally identified by LC-MS, ESI positive ion mode scanning analysis. Results A total of 13 main chemical constituents were detected according to the MS data of each chromatographic peak obtained in positive ion mode. Three of them were confirmed by comparison with literature or by mass spectrometry. They were valine, adenine , Arginine; Compounds 1, 2, 4, 5, 7, 8 and 13 were inferred to be 5-hydroxymethylfurfural, 6 H-purin-6-1,2- (1-naphthalenylamino), cyclo- (valine-tyrosine), cyclo- (leucine-tyrosine), leucine- isoleucine, (-) - pohakulin pohakuline, - (phenylacetyl) -L-prolyl) glycine ethyl ester, Compound 9 is presumed to be a cyclic peptide. Compounds 10 and 11, due to the lack of related reference substance and related literature, have to be further elucidated for their structures. Conclusion The material that eluted out of the C18 column during the dead time and did not separate well was further separated on the packed column, suggesting that to some extent some of the compounds that do not separate well with a single stationary phase can be mixed For the further separation of the stationary phase chromatographic column, especially in the separation and identification of complex system samples, the mixed stationary phase chromatographic column will have good application prospects.