吴茱萸次碱的制备方法  

Preparation method of rutaecarpine

作　　者：李琦[1] 曹青云[1] 肖顺丽 王敏[1] 关亮俊 张宏桂[2] 

机构地区：[1]北京中医药大学中药学院,2015级硕士研究生北京100102 [2]北京中医药大学中药学院科技发展部,北京100102

出　　处：《河北中医》2017年第3期439-443,共5页Hebei Journal of Traditional Chinese Medicine

基　　金：国家自然科学基金资助项目(编号:30870262)

摘　　要：目的以吴茱萸为原料,研究简单、快速、高效的分离、纯化吴茱萸次碱的制备方法。方法采用85%乙醇提取,硅胶柱层析分离,甲醇重结晶纯化吴茱萸次碱,薄层鉴别(TLC)、高效液相色谱法(HPLC)、核磁方法检查纯度。结果吴茱萸次碱经TLC检查与对照品一致,无杂质斑点,经HPLC检测纯度达98.5%以上,经核磁鉴定。另外经考察,确定色谱条件为Waters C18柱(150 mm×4.6 mm,5μm);检测波长225、290、215、365 nm;流动相乙腈-水溶液(50∶50);进样量10μL;柱温35℃;体积流量1.0 m L/min。结论吴茱萸次碱对照品已达到中药质量检测用化学对照品技术要求,所采取的分离、纯化方法简单、安全、可行性强,成本低、效率高,可用于吴茱萸药材及其制剂的质量控制。Objective Using evodia as the material,to study a simple,rapid and efficient preparation method for the separation and purification of rutaecarpine. Methods The rutaecarpin were prepared by using 85% ethanol extraction,silica-gel column chromatography separation and methanol recrystallization purification. The purity was checked by thin layer identification（ TLC）,high performance liquid chromatography（ HPLC） and nuclear magnetic resonance（ NMR）. Results Rutaecarpine was consistent with the reference substance upon TLC,without impurities and spots,the purity over 98. 5% upon HPLC,which identified by NMR. In addition,the chromatographic conditions were determined as Waters C18column（ 150 mm × 4. 6 mm,5 μm）,determine wavelengths： 225,290,215,365 nm; moving phase： acetonitrile-aqueous solution（ 50∶ 50）; sample size： 10 μL; column temperature： 35℃; volume flow rate： 1. 0 m L/min. Conclusion Rutaecarpine reference substance has reached the technical requirements of Traditional Chinese medicine with chemical reference materials,the method for separation and purification is simple,safe,strong feasibility,low cost,high efficiency,can be used for the quality control of evodia medicinal materials and its preparations.

关 键 词：生物碱类 吴茱萸 化学 制备 

分 类 号：R282.71[医药卫生—中药学] R284.1[医药卫生—中医学]