基于超高效液相色谱分析黄连、吴茱萸配伍药对的有效成分

Effective Components of Rhizoma Coptidis and Fructus Evodiae Compatibility Based on Ultra-high Performance Liquid Chromatography

目的:评价通过超高效液相色谱(UPLC)分析黄连、吴茱萸配伍药对的有效成分。方法:选取4对不同产地的黄连、吴茱萸配伍药对进行研究,采用ACQUITY UPLC BEH C18作为本研究的色谱柱(1. 7μm,100 mm×2. 1 mm),柱温为40℃;加入2μL10℃的样品后,以乙腈(流动相A)-纯水加0. 05%甲酸(流动相B),流速为0. 4 m L/min进行梯度洗脱,建立UPLC-质谱(MS)指纹图谱分析方法。结果:在黄连、吴茱萸配伍药对的对照指纹图谱和样品指纹图谱的比较中,相对保留时间标定16个较有特征的共有峰分别与单味黄连药物及单味吴茱萸的指纹图谱特征峰比较,发现9、15和16号共有峰是黄连、吴茱萸都存在的特征峰,而1、2、13、14号共有峰仅吴茱萸方有的特征峰,余下共有峰为黄连药物的特征峰。9、15和16号黄连、吴茱萸配伍药对共有的特征峰,结合质谱分析和化合物质裂解规律,推测出木兰花碱、格陵兰黄连碱和1-甲基-2壬基-4(1H)-奎若酮等3中化合物。结论:采用UPLC-MS技术建立黄连、吴茱萸配伍药对有效成分,为黄连和吴茱萸药材的有效成分和质量评估提供参考。

Objective：To analyze the effective components of Rhizoma Coptidis and Fructus Evodiae compatibility by ultra-high performance liquid chromatography（UPLC）. Methods ：A total of 4 pairs of different origin of the compatibility of Rhizoma Coptidis and Fructus Evodiae. ACQUITY UPLC BEH C18 was used as a colunm of this study（ 1.7 μm, 100 mm × 2. 1 mm）. The colunm temperature was 40℃. 2 μl L 10℃ after samples with acetonitrile（ mobile phase A） -water with 0. 05 % formic acid（ mobile phase B） was added. The flow rate was 0. 4 mL/nfin by gradient elution. UPLC-mass spectrometry（MS） fingerprint analysis method was established. Results：1）In the combination of Rhizoma Coptidis and Fruetus Evodiae compatibility, control fingerprint and sample fingerprint were compared according to the relative retention time calibration of 16 more characteristic common peaks. The 16 peaks were respectively compared with the fingerprint of Rhizoma Coptidis characteristic peaks and Fruetus Evodiae fingerprint character- istic peaks. Rhizoma Coptidis and Fruetus Evodiae shared 9,15, and 16 characteristic peaks. The 1,2,13,14 common peaks were presented in Fruetus Evodiae characteristic peaks. The rest peaks was presented in Rhizoma Coptidis. 2）Effective components of the combination of Rhizoma Coptidis and Fruetus Evodiae were qualitatively analyzed using UPLC and mass spectrometry analysis. Rhizoma Coptidis and Fruetus Evodiae shared 9,15 and 16 common characteristic peaks were showed in Table 2. Magnoflorine Greenland,eoptisine and 1-methyl nonyl-2-4 （1H）-Quirrell ketone compounds were inferred with mass spectrometry and compounds cracking law. Conclusion ：The effective components of Rhizoma Coptidis and Fruetus Evodiae compatibility was established by UP- LC-MS technology, providing reference for effective components and quality evaluation of Rhizoma Coptidis and Fruetus Evodiae.