摘要
目的建立左金丸组分中药配伍组分制备工艺并对所得组分的主要成分进行定性和定量表征。方法通过正交试验设计考察最佳提取溶剂、提取时间和提取次数;以总生物碱含量为指标考察吸附树脂类型、最佳上样质量浓度、上样量、径高比和吸附时间;采用超高效液相色谱-串联质谱法(UPLC-MS/MS)和UPLC法对组分中的主要成分进行定性和定量分析。结果所选工艺流程为10倍量70%乙醇回流提取2次,每次1 h;提取物用AB-8大孔树脂柱纯化,最佳上样质量浓度为0.5 g/mL,上样量为0.12个柱体积(BV),径高比为1∶12,吸附时间为1 h;洗脱溶剂依次为28 BV 40%乙醇,16 BV 60%乙醇,13 BV 95%乙醇。上述工艺流程得到3个组分,即C40、C60和C95组分。从C40组分中指认了31个成分,主要为黄连生物碱类,其中盐酸小檗碱含量最高(20.15%);从C60组分中指认了32个成分,主要为吴茱萸柠檬苦素类,其中柠檬苦素含量最高(15.40%);从C95组分指认了36个成分,主要为吴茱萸生物碱类,其中吴茱萸次碱含量最高(4.14%)。结论建立的左金丸组分中药配伍组分制备工艺重复性好,所得组分活性成分含量高,质量稳定,为进一步成药性研究和组分中药研制奠定基础。
Objective To establish the preparation process of components for component-based Chinese medicine of Zuojin Pills(左金丸)and analyze the main compounds of components qualitatively and quantitatively.Methods Orthogonal experimental design was employed to determine the optimal extracting solvent,extracting time and extracting times.The resin type,optimum loading concentration,loading quantity,diameter-height ratio and adsorption time were investigated using total alkaloid content as index.The qualitative and quantitative analysis of main compounds were conducted by ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)and UPLC,respectively.Results The selected process was that the powders were extracted with 10 folds of 70%ethanol under reflux two times for 1 h each.AB-8 macroporous resin was selected to purify the extracts.The optimum loading concentration was 0.5 g/mL,loading volume was 0.12 BV,diameter-height ratio was 1:12 and adsorption time was 1 h.The elution was carried out with 28 BV 40%ethanol,16 BV 60%ethanol and 13 BV 95%ethanol successively to obtain three components,C40,C60 and C95 components.Thirty-one compounds,which were mainly alkaloids from Coptidis Rhizoma(Huanglian),were identified from C40 component.Among them,the content of berberine was the highest(20.15%).Thirty-two compounds,which were mainly limonoids from Evodiae Fructus(Wuzhuyu),were identified from C60 component.Among them,the content of limonin was the highest(15.40%).Thirty-six compounds,which were mainly alkaloids from Evodiae Fructus,were identified from C95 component.Among them,the content of rutaecarpine was the highest(4.14%).Conclusion The preparation process established herein is repeatable and the resultant components with high content of active compounds are qualitive stable.This study lays a foundation for further research and development of druggability and component-based Chinese medicine of Zuojin Pills.
作者
刘斯琪
王如峰
LIU Si-qi;WANG Ru-feng(School of Life Sciences,Beijing University of Chinese Medicine,Beijing 102488,China)
出处
《中草药》
CAS
CSCD
北大核心
2022年第19期6001-6011,共11页
Chinese Traditional and Herbal Drugs
基金
国家重点研发计划(2018YFC1704506)。
关键词
左金丸
黄连
吴茱萸
组分中药
UPLC-MS/MS
生物碱
盐酸小檗碱
柠檬苦素
吴茱萸次碱
Zuojin Pills
Coptidis Rhizoma
Evodiae Fructus
component-based Chinese medicine
UPLC-MS/MS
alkaloids
berberine hydrochloride
limonin
rutaecarpin
