论文部分内容阅读
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 establish a HPLC-ESI-MS / MS method for the determination of the chemical constituents in KunTai Capsules. The chemical constituents were identified preliminarily. Methods: The constituents of Kuntai capsule were elucidated by LC-ESI-MS / MS. The mobile phase consisted of C18 column (4.6 mm × 150 mm, 5 μm) and acetonitrile-0.1% formic acid , The flow rate was 1.0 mL · min ~ (-1) and the column temperature was 30 ℃. Mass Spectrometry Electrospray (ESI) ion source was used to collect data in positive ion mode. Quality scan range of m / z 50 ~ 1 500. The chromatograms of each peak were analyzed, and the relative molecular mass was determined according to the peak of quasi- ion ion. The structure of the compound was further deduced from the literature data by the information of the major fragment ion, UV spectrum and retention time. RESULTS: Twenty-one compounds were identified from Kuntai capsules, mainly flavonoids and alkaloids, and the medicinal materials of the compounds were assigned. Among them, there are baicalin from baicalin, baicalin, baicalein, wogonin and so on, from the Coptis Palmatine, berberine, berberine, jatrorrhizine, tetrandrine, etc. come from Paeoniflorin and other white peony root. Conclusion: The main constituents in Kuntai Capsules can be rapidly analyzed and identified by LC-ESIMS / MS, which lays the foundation for the further study on the fingerprint, quality control, drug metabolism and spectrum-efficiency of Kuntai Capsules.