CAJ | 학술논문

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（150 mm ×4．6 mm ，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 ，150 mm ×2．0 mm ，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。
목적대중약반하중재C18색보주상보류교약적화학성분진행분리여감정。방법수선채용Waters X‐Bridge C18색보주（150 mm ×4．6 mm ，5μm）대반하약재산수제취액진행분리，연후대반하제취액중재C18주상보류교약적성분채용Tech Mate TX색보주（120A ，150 mm ×2．0 mm ，5μm）（SCX여반상C18혼합전료색보주）진행진일보분리분석，최후채용LC‐MS대소분리성분진행감정，ESI정리자모식소묘분석。결과근거정리자모식하획득적각색보봉적질보수거，공검측도13개주요적화학성분，기중3개통과여문헌대조혹근거질보렬해규률득도료학인，분별위：힐안산，선표령，정안산；화합물1，2，4，5，7，8화13추측위：5‐간갑기강철，6 H‐purin‐6‐1，2‐amino‐1，9‐dihydro‐8‐（1‐naphthalenylamino），배‐（힐안산‐락안산），배‐（량안산‐락안산），량안산‐이량안산，（－）‐pohakulin pohakuline ，N‐（1‐（분기을선기）‐L‐포안선）감안산을지，화합물9추측위모충배태；화합물10화11유우결핍상관대조품화상관문헌보도，기결구유대진일보분석감정。결론재C18주상사시간내류출이불능흔호분리적물질，재혼합전료주상득도료진일보분리，저설명재모충정도상，채용단일고정상불능흔호분리적모사화합물가이채용혼합고정상색보주체도진일보분리，우기시재대복잡체계양품적분리급감정과정중，혼합고정상색보주장구유량호적응용전경。
Objective To separate and identify the chemical compositions of Pinellia ternate which is slightly reserved on the C18 col‐umn .Methods Firstly a Waters X‐Bridge C18 column was used to separate the acidic water extract of Pinellia ternate ,and then the Tech MateTX column (120A ,150 mm × 2 .0 mm ,5 μm) (SCX‐C18 mixed stationary phase column) was used to separate the components that slightly retained on the C18 column ,and finally the components that slightly retained on the C18 column were sepa‐rated and identified by LC‐MS‐ESI in a positive ion mode .Results According to the positive ion mode available mass spectral data for each chromatographic peak ,13 major chemical constituents were detected ,3 of which were confirmed by literature or under the control of MS fragmentation mechanism .They were adenine ,valine ,and arginine .Compounds 1 ,2 ,4 ,5 ,7 ,8 and 13 were:5‐hydroxymethyl furfural ,6 H‐purin‐6‐1 ,2‐amino‐1 ,9‐dihydro‐8‐(1‐naphthalenylamino) ,ring‐(Val Tyr) ,cyclo(leu‐tyr) ,leucine‐iso‐leucine ,(-)‐pohakulinpohakuline ,and N‐(1‐(phenylacetyl)‐L‐prolyl)glycine ethyl ester .Compound 9 was presumed to be a cyclic peptide;due to the lack of control and related literatures ,the structure of compounds 10 and 11 need to be identified for further a‐nalysis .Conclusion The substances which were flowed out in the dead time on the C18 column can be separated on the mixed‐sta‐tionary phase column .The mixed‐stationary phase will has a good application prospects .