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目的建立超高效液相色谱-飞行时间质谱联用法(UPLC-Q-TOF-MS)快速鉴定淫羊藿饮片中的化学成分。方法采用Waters Acquity UPLC BEH C18(100 mm×2.1 mm,1.7μm)色谱柱,以0.1%甲酸水溶液(A)-0.1%甲酸乙腈溶液(B)为流动相进行梯度洗脱,体积流量0.4 m L/min,柱温35℃,进样量5μL。质谱采用电喷雾(ESI)离子源,在负离子模式下采集数据,通过保留时间、精确相对分子质量和二级质谱碎片对检测到的化学成分进行鉴定。结果检测到淫羊藿饮片中以脱水淫羊藿素为母核的黄酮类成分17个、以去甲基脱水淫羊藿素为母核的黄酮类成分6个、其他类型化合物6个。再通过分析10批样品中的化学成分,确定了淫羊藿饮片中16个普遍存在的化学成分。结论 UPLC-Q-TOF-MS方法能快速、准确、较全面地鉴定淫羊藿饮片中的化学成分;淫羊藿化学成分的鉴定及普遍存在化学成分的确定为其药效物质基础和质量控制研究提供了实验依据。
OBJECTIVE To establish a rapid HPLC-Q-TOF-MS method for the determination of chemical constituents in Epimedium Tablets. Methods A gradient elution was performed on a Waters Acquity UPLC BEH C18 (100 mm × 2.1 mm, 1.7 μm) column using 0.1% formic acid in water (A) and 0.1% formic acid in acetonitrile (B) / min, column temperature 35 ℃, injection volume 5μL. Mass spectrometry The electrospray (ESI) ion source was used to collect data in negative ion mode and the chemical composition detected was identified by retention time, exact relative molecular mass and secondary mass fraction. Results Seventeen flavonoids were isolated from epimedium slices and 6 were flavonoids with demethyl ictidine as the mother nucleus and 6 other types of compounds. Then by analyzing the chemical composition of 10 batches of samples to determine Epimedium Pieces of 16 common chemical composition. Conclusion The UPLC-Q-TOF-MS method can rapidly, accurately and completely identify the chemical constituents of Epimedium Pieces. The chemical constituents identification and ubiquitous chemical constituents determination of Epimedium are the basis and quality control The research provided the experimental basis.