Key Laboratory of Combinatorial Biosynthesis and Drug Discovery, Ministry of Education, and Wuhan University School of Pharmaceutical Sciences, Wuhan, 430071, China; State Key Laboratory of Transducer Technology, Chinese Academy of Sciences, Beijing 10080, China.
Key Laboratory of Combinatorial Biosynthesis and Drug Discovery, Ministry of Education, and Wuhan University School of Pharmaceutical Sciences, Wuhan, 430071, China.
J Chromatogr A. 2019 Sep 27;1602:474-480. doi: 10.1016/j.chroma.2019.06.011. Epub 2019 Jun 5.
Evodiae Fructus is used as a traditional Chinese medicine for the treatment of several kinds of diseases with its bioactive constituents. In this study, a capillary electrochromatography-mass spectrometry (CEC-MS) method was developed to determine three bioactive compounds including evodiamine, rutaecarpine and limonin in Evodiae Fructus fruit. Home-developed monolithic columns with methyl-vinylimidazole functionalized organic polymer monolilth as stationary phases were used in CEC-MS with excellent separation selectivity and high efficiency. The CEC-MS methods provided 4-16 folds improvement of LODs when compared with CEC-UV method. The conditions, which could affect separation efficiency and detection sensitivity, were optimized. Under optimum conditions, baseline separation with high detection sensitivity was obtained. The method showed good linearity (R >0.99) of 0.8-160 μg mL with low limits of detection of 0.15-0.31 μg mL. Relative standard deviations of migration time and relative peak areas were <13.89%. Recoveries of evodiamine, rutaecarpine and limonin in Evodiae Fructus fruit were tested and calculated, which ranged from 102% to 113%. Finally, the three bioactive compounds in Evodiae Fructus herb samples from different regions were analyzed and studied. It has been demonstrated that the developed method has great potential for quality control of Evodiae Fructus herb.
吴茱萸作为一种传统中药，其生物活性成分被用于治疗多种疾病。本研究建立了毛细管电色谱-质谱（CEC-MS）法测定吴茱萸果实中三种生物活性成分吴茱萸碱、吴茱萸卡品碱和柠檬苦素的含量。采用自制的以甲基-乙烯基咪唑功能化有机聚合物为固定相的整体柱，在 CEC-MS 中具有优异的分离选择性和高效性。与 CEC-UV 方法相比，CEC-MS 方法的检出限提高了 4-16 倍。优化了分离效率和检测灵敏度的影响条件。在最佳条件下，实现了基线分离和高检测灵敏度。该方法的线性范围为 0.8-160μg/mL（R>0.99），检出限为 0.15-0.31μg/mL。迁移时间和相对峰面积的相对标准偏差均<13.89%。吴茱萸果实中吴茱萸碱、吴茱萸卡品碱和柠檬苦素的回收率在 102%-113%之间。最后，对不同产地吴茱萸药材样品中的三种生物活性成分进行了分析研究。结果表明，该方法可用于吴茱萸药材的质量控制。
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