Zhao Liang, Lou Zi-Yang, Zhu Zhen-Yu, Zhang Guo-Qing, Chai Yi-Feng
Department of Pharmaceutical Analysis, School of Pharmacy, Second Military Medical University, and Department of Pharmacy, Eastern Heptatobiliary Surgery Hospital, Shanghai 200433, People's Republic of China.
Biomed Chromatogr. 2008 Jan;22(1):64-72. doi: 10.1002/bmc.897.
A reliable and rapid method based on rapid-resolution liquid chromatography-diode array detection (RRLC-DAD) and electrospray ionization time-of-flight mass spectrometry (ESI-TOF/MS) has been developed for the isolation and characterization of multiple constituents in the root of Stellera chamaejasme L., which was extracted by sonication with methanol in an optimized procedure. Separation of the multiple constituents was achieved on an Agilent Zorbax XDB-C18 (50x3.0 mm i.d.; 1.8 microm) column using a gradient elution at a flow rate of 0.4 mL/min. The detection wavelength was 210 nm. Mass spectra were acquired in both positive and negative modes. A formula database of the known chemical constituents in the root of Stellera chamaejasme L. was established by an Agilent software. Twenty-two obvious peaks appeared in the total ion chromatogram and nine of them were characterized by TOF/MS. The RRLC-DAD and ESI-TOF/MS method with ultrasonic extraction would be useful for rapid and effective characterization of chemical constituents in the root of Stellera chamaejasme L.
基于快速分离液相色谱 - 二极管阵列检测(RRLC - DAD)和电喷雾电离飞行时间质谱(ESI - TOF/MS),已开发出一种可靠且快速的方法,用于瑞香狼毒根中多种成分的分离与表征。该根采用优化的甲醇超声提取程序进行提取。多种成分在安捷伦Zorbax XDB - C18(内径50×3.0 mm;1.8微米)柱上以0.4 mL/min的流速进行梯度洗脱分离。检测波长为210 nm。质谱以正离子和负离子模式采集。通过安捷伦软件建立了瑞香狼毒根中已知化学成分的分子式数据库。总离子色谱图中出现了22个明显的峰,其中9个通过TOF/MS进行了表征。RRLC - DAD和ESI - TOF/MS方法结合超声提取,将有助于快速有效地表征瑞香狼毒根中的化学成分。