本研究报道了一种制备人面果中π键二苯甲酮异构体环大叶藤黄醇和异大叶藤黄醇的液相色谱研究方法.实验中通过色谱柱以及流动相考察,在分析色谱柱上实现了液相方法的建立、模拟及筛选试验,并在半制备色谱柱上实现了放大试验和进样量考察.优化后的色谱条件可实现异构体达到2.5的分离度,并在浓度0.2 μg/μL时的进样量达到500 μL,单体化合物环大叶藤黄醇和异大叶藤黄醇可通过液相色谱、核磁共振DEPT谱及质谱予以确认.该研究表明,常规C18色谱柱能够对π键异构体进行拆分,将加快更多具有生物活性的二苯甲酮单体化合物的发现.%This study reported a liquid chromatographic method for preparing π-bond benzophenone isomers cycloxanthochymol and isoxanthochymol from Garcinia xanthochymus.The liquid chromatographic method was proposed,simulated and optimized through column selection and buffer selection on analytical columns,and verified on a preparative column.Cycloxanthochymol and isoxanthochymol were prepared after the inject volume selection,and identified by NMR as well as mass spectrometry.The optimized method realized baseline separation with resolution of 2.5,and the isomers were prepared with the inject volume of 500 μL at sample concentration of 0.2 μg/μL.Results of the HPLC analysis and the distortionless enhancement by polarization transfer confirmed the differences between the monomers on the π bond position.In conclusion,this study indicated that a common octadecyl bonded silica gel column can meet the challenge preparation of π bond isomers,which will accelerate the foundation of more bioactive benzophenone compounds in the future.
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