基于UPLC-Q-TOF-MS的淫羊藿化学成分分析  

Analysis on chemical constituents of Epimedii Folium by UPLC-Q-TOF-MS

作　　者：王媛[1] 袁磊[1] 李遇伯[1] 张艳军 WANG Yuan YUAN Lei LI Yu-bo ZHANG Yan-jun(School of Chinese Materia Medica, Tianjin University of Traditional Chinese Medicine, Tianjin 300193, China Tianjin state key laboratory of modem Chinese medicine, Tianjin 300193, China)

机构地区：[1]天津中医药大学中药学院,天津300193 [2]天津市省部共建现代中药重点实验室,天津300193

出　　处：《中草药》2017年第13期2625-2631,共7页Chinese Traditional and Herbal Drugs

基　　金：国家科技支撑计划(2011BAI07B00)

摘　　要：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 quick method of ultra-performance liquid chromatography-quadruple time-of-fight mass spectrometry（UPLC-Q-TOF-MS） for the identification of chemical constituents in Epimedii Folium. Methods The separation was performed on the chromatographic column of Waters Acquity UPLC BEH C18（100 mm × 2.1 mm, 1.7 μm）. The mobile phase consisted of 0.1% formic acid-water（A） and 0.1% formic acid-acetonitrile（B） was used as gradient elute. The flow rate was 0.4 m L/min gradient elution and column temperature was 35 ℃. The injection volume was 5 μL. The negative ion mode was used for TOF-MS scanning. The compounds were identified by retention time, accurate relative molecular mass, and fragment ions in mass spectrometry. Results Based on the MS/MS of standards and compared with reference results, 29 compounds were discovered. Then 10 batches of Epimedii Folium sample were analyzed, and compounds in them were also identified. Finally, 16 constituents exiting in all samples were found. Conclusion The results demonstrate that UPLC-Q-TOF-MS method is quick, accurate, and efficient for the identification of the compounds in Epimedii Folium. The identification of chemical compositions and the definition of compositions generally existed in Epimedii Folium which provides some experiment foundation for study of its efficiency substances and quality control.

关 键 词：淫羊藿 超高效液相色谱-飞行时间质谱 黄酮类 脱水淫羊藿素 去甲基脱水淫羊藿素 

分 类 号：R284.1[医药卫生—中药学]