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射干异黄酮类化学成分的HPLC-DAD/ESI-MS分析
冯超,周婷婷,范国荣*,魏华
0
(第二军医大学药学院药物分析学教研室,上海 200433)
摘要:
目的:通过高效液相色谱-二极管阵列光谱检测/电喷雾离子化质谱(HPLC-DAD/ESI-MS)联用技术定性分析射干中的主要化学成分。方法:以70%乙醇超声辅助提取中药射干原药材。高效液相色谱条件:选择YMC ODS-C18 (250 mm×4.6 mm I.D.,5 μm)色谱柱,以20%甲醇水溶液A-70%乙腈水溶液B(0→30→45→65 min,20%→30%→90%→100% B)梯度洗脱,流速为0.45 ml/min,检测波长为265 nm。ESI质谱条件:正离子扫描模式,喷针电压5 000 V,毛细管电压 20 V,干燥气(N2)压力20 psi(1 psi=6 894.8 Pa),质量扫描范围m/z 250~550,雾化温度 300℃。结果:通过 HPLC-DAD/ESI-MS联用技术,分离检测并鉴定出射干中9个主要异黄酮类化学成分。结论:通过 HPLC-DAD/ESI-MS联用技术,为鉴定射干中的化学成分建立起了一种快速、高效的分析方法,也为中药射干的质量控制提供更多的科学依据。
关键词:  射干  高效液相色谱-二极管阵列光谱检测/电喷雾离子化质谱联用  化学成分
DOI:10.3724/SP.J.1008.2009.0817
投稿时间:2008-12-17修订日期:2009-04-11
基金项目:
HPLC-DAD/ESI-MS in analyzing chemical constituents of Rhizoma belamcanda
FENG Chao,ZHOU Ting-ting,FAN Guo-rong* ,WEI Hua
(Department of Drug Analysis,School of Pharmacy,Second Military Medical University,Shanghai 200433,China)
Abstract:
Objective:To analyze the chemical constituents of Rhizoma belamcandae by using high-performance liquid chromatography-diode array detector/electrospray ionization-mass spectrometry (HPLC-DAD/ESI-MS).Methods: Dried Belamcanda chinensis powder was extracted with 70% ethanol by sonication.The chromatographic separation was performed on a YMC ODS-C18 column (250 mm×4.6 mm I.D.,5 μm) with a mobile phase composed of 20%CH3OH(A)-70%ACN(B) (0→30→45→65 min,20→30→90→100 B),eluted at a flow rate of 0.45 ml/min,and the UV detection wavelength was set at 265 nm.Positive ionization mode with a needle voltage of 5 000 V,a capillary voltage of 20 V,a gas(N2)press of 20 psi and a temperature of the drying gas of 300℃ was selected.Relative molecular mass data acquisition was performed from m/z 250 to 550 in full MS scan mode.Results: Nine major isoflavones were identified from Rhizoma belamcandae based on their retention behavior obtained on-line by their UV spectra and the HPLC-DAD/ESI-MS.Conclusion: A rapid and efficient HPLC-DAD/ESI-MS method for identifying the chemical constituents of Belamcandae chinensis has been established,which provides more scientific information for quality control of Rhizoma belamcandae.
Key words:  Belamcandae chinensis  HPLC-DAD/ESI-MS  chemical constituents