目的:对甘地胶囊的化学成分进行快速分离与鉴别。方法:采用高效液相色谱.电喷雾.高分辨飞行时间质谱(HPLCESI—TOF/MS)联用技术。色谱柱为Agilent Poroshell 120 SB-C18(100mm×3mm,2.7μm),流动相为0.1%甲酸水溶液.乙腈(梯度洗脱),流速为0.4ml/min,检测波长为254nm,柱温为25℃,进样量为10μl;使用ESI离子源,在负离子模式下采集数据,N2流速为10L/min,载气温度为350℃,毛细管电压为4000V,轰击电压为165V,扫描质量范围(m/z)为100~1100amu。结果:推断出甘地胶囊内容物中主要成分有18种,分别为8-表马钱子苷酸、莫诺苷、马钱素、当药苷、芦丁、异毛蕊花苷、山柰酚-3-O-芸香糖苷、山茱萸新苷、黄芩苷、山柰酚-3-O-葡糖苷、2’-羟基-3',4’-二甲氧基异黄烷-7-O-β-d-葡糖苷、汉黄芩苷、黄芪甲苷、黄芩素、汉黄芩素、黄芩新素Ⅱ、异黄芪皂苷Ⅰ、乙酰黄芪皂苷Ⅰ。结论:该方法快速、微量、高效,可为甘地胶囊的药效物质基础和质量控制研究奠定基础。
OBJECTIVE: To separate and identify the chemical constituents of Gandi capsule. METHODS: HPLC-ESI-TOF/ MS was adopted. The determination was performed on Agilent Poroshell 120 SB-C18(100 mm×3 mm, 2.7 μm) column with mobile phase consisted of 0.1% formic acid-acetonitrile (gradient elution) at the flow rate of 0.4 ml/min. The detection wavelength was set at 254 nm, and column temperature was 25℃. The sample size was 10 μl. ESI and negative ion mode were adopted, and the flow rate and temperature of carrier gas (N2) were 10 L/min and 350℃, respectively. The capillary voltage was 4 000 V, the bombardment voltage was 165 V, and scanning proton range were 100-1 100 amu. RESULTS: A total of 18 chemical constituents were identified in Gandi capsule, including 8-epiloganic acid, morroniside, loganin, sweroside, rutin, isoverbascoside, kaempferol 3-rutinoside, cornuside, baicalin, kaempferol-3-glucoside, 2'-Hydroxy-3', 4'-dimethoxy-isoflavane-7-O-β-d-glucoside, wogonoside, astragaloside, baicalein, wogonin, skullcapflavon Ⅱ, isoastragaloside Ⅰ and acetytastragaloside Ⅰ. CONCLUSIONS: The method is rapid, trace and highly active, and can lay foundation for pharmacodynamic material basis and quality control of Gandi capsule.