【作者】 殷月芬； 陈军辉； 杨佰娟； 李文龙； 黎先春； 王小如；

【Author】 YIN Yue-fen1,2,CHEN Jun-hui1,2, YANG Bai-juan2, LI Wen-long2, Frank Sen-Chun Lee 2,Wang Xiao-ru2,3* (1. College of Chemistry and Chemical Engineering, Ocean University of China, Qingdao 266003; 2. QingDao Key Lab on Analytical Technology Development and Standardization of Chinese Medicines, First Institute Oceanography of SOA, Qingdao, 26606; 3. Department of Chemistry and the Key Laboratory of Analytical Science of the MOE, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005, China)

【机构】 中国海洋大学化学化工学院； 国家海洋局第一海洋研究所青岛现代分析技术及中药标准化重点实验室；

【摘要】 目的采用高分辨电喷雾飞行时间质谱(ESI-TOF-MS)联用技术,对片蟾酥中的部分成分进行了初步鉴定,探讨HPLC-ESI-TOF-MS联用技术作为蟾酥质量控制方法的可行性。方法采用Agilent C18色谱柱,以甲醇和水(含0.1磷酸)为流动相洗脱,流速为1.0ml/min,室温,DAD检测器检测波长为291nm,ESI-TOF-MS采用正离子模式。通过HPLC-ESI-TOF-MS在线测定部分化合物的精确分子量,结合文献报道,初步鉴定蟾毒素。结果在主要色谱峰当中,可以确定其中的3个峰是已有文献报道的化合物。结论高效液相色谱-电喷雾飞行时间质谱法和作为蟾酥质量控制的方法。更多还原

【Abstract】 OBJECTIVE To identify the active components in Venenum Bufonis by high performance liquid chromatography (HPLC)- electrospray –time of flight mass spectrometry (ESI-TOF-MS). METHODS The separation was performed on a Agilent Eclipse XDB C18 (4.6 mm×150 mm) column with gradient elution of methanol and water (with 0.1% phosphoric acid) as mobile phase, flow-rate is 1.0ml/min,at room temperature (about 25 ℃). The detection wavelength is 291 nm and the UV spectra of peaks were obtained with a photodiode array detector (DAD). On-line ESI-TOF-MS in positive mode was used to get the mass spectrum of some of the analytes. RESULTS Three effective components in Venenum Bufonis were primarily identified by comparison of the UV spectra and mass spectrum with literature. CONCLUSION HPLC-ESI-TOF-MS is a very powerful tool for identification the effective components in Venenum Bufonis更多还原