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机构地区:[1]上海海天医药科技开发有限公司,上海200023 [2]中国药科大学,南京210009 [3]上海中医药大学,上海201203
出 处:《中国实验方剂学杂志》2017年第19期90-93,共4页Chinese Journal of Experimental Traditional Medical Formulae
基 金:贵州省科技计划项目(黔科合[2016]支撑2821)
摘 要:目的:建立坤泰胶囊中化学成分的高效液相色谱-电喷雾质谱联用技术(HPLC-ESI-MS/MS)并对其化学成分进行初步鉴定。方法:采用LC-ESI-MS/MS对坤泰胶囊进行成分分析与鉴定,选用C_(18)色谱柱(4.6 mm×150 mm,5μm),以乙腈-0.1%甲酸水溶液为流动相梯度洗脱,流速1.0 mL·min^(-1),柱温30℃。质谱使用电喷雾(ESI)离子源,正离子模式采集数据。质量扫描范围为m/z 50~1 500。对各色谱峰质谱图进行分析,根据准分子离子峰判断相对分子质量,进一步根据各主要碎片离子、紫外光谱、保留时间等信息,与文献数据进行比较推测化合物的结构。结果:从坤泰胶囊中鉴定了21个化合物,主要为黄酮类化合物和生物碱类化合物,并对化合物的药材来源进行了归属。其中,主要有来自黄芩的黄芩苷、汉黄芩苷、黄芩素、汉黄芩素等,来自黄连的巴马汀、小檗碱、黄连碱、药根碱、非洲防己碱、木兰花碱等,来自白芍的芍药苷等。结论:采用LC-ESIMS/MS能够对坤泰胶囊中主要成分进行快速分析与鉴定,为坤泰胶囊进一步开展指纹图谱、质量控制、药物代谢研究和谱效关系研究奠定了基础。Objective: To identify the chemical constituents of Kuntai capsule by high performance liquid chromatography with electrospray ionization tandem mass spectrometry (HPLC-ESI-MS/MS). Method: The chemical components were analyzed and identified by using LC-ESI-MS/MS. The liquid chromatography separation was carried out on C18 column (4.6 mm×150 mm, 5 μm) with acetonitrile-0.1% formic acid solution as the mobile phase for gradient elution. The flow rate was 1.0 mL·min^-1 and column temperature was 30℃. The mass spectra were obtained in positive ion mode with electrospray ionization. The mass range recorder was set between m/z 50-1 500.The molecular weight was determined according to the molecular ion peaks. The compound structures were elucidated by comparing the data with literature data,including main ion peaks, UV spectrum and HPLC retention time information. Result: The 21 compounds were identified from Kuntai capsule, mainly including flavones and alkaloids. The flavones, such as baicalin, wogonoside, baicalein and wogonin, were identified from Scutellaria baicalensis. The alkaloids, such as palmatine, berberine, coptisine, jatrorrhizine, columbarine and magnoflorine, were identified from Coptis chinensis; paeoniflorin came from Paeonia lactiflora. Conclusion: The method is simple and rapid for identifying the main constituents of Kuntai capsule. This paper has laid a foundation for further studying and testing the quality of Kuntai capsule.
关 键 词:坤泰胶囊 化学成分 生物碱 黄酮 高效液相色谱-电喷雾质谱
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