中国中药杂志

2011, v.36(02) 169-174

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续断的色谱指纹及LC-ESI-MS分析
Chromatographic fingerprint of Dipsacus asper and analysis by HPLC-MS

韦英杰;贾晓斌;樊宏伟;彭蕴茹;詹雯;
WEI Yingjie1,JIA Xiaobin1,FAN Hongwei2,PENG Yunru1,ZHAN Wen1(1.Key Laboratory of New Drug Delivery System of Chinese Meteria Medica,Jiangsu ProvincialAcademy of Chinese Medicine,Nanjing 210028,China;2.Lab of Clinical Pharmacology,Affiliated Nanjing First Hospital,Nanjing Medical University,Nanjing 210006,China)

摘要(Abstract):

目的:建立中药续断高效液相指纹图谱,分析色谱峰的化合物类型和质谱特征,提高续断的质量控制水平。方法:采用高效液相色谱-二极管阵列检测器(HPLC-DAD),Zorbax Extend C18(4.6 mm×150 mm,5μm)色谱柱,乙腈-0.1%磷酸水梯度洗脱,以川续断皂苷VI为参照物,建立续断色谱指纹。通过二极管阵列检测分析色谱指纹峰的化合物类型,采用液相色谱与电喷雾质谱联用技术首次分析了续断化学成分的质谱特征。结果:确定24批续断药材的17个共有峰,该指纹图谱具有良好的精密度、稳定性和重复性,成功用于24批续断药材的质量评价。二极管阵列检测区分了续断皂苷和非皂苷类化合物的指纹峰,液相色谱与质谱联用技术鉴定了30多个化合物的相对分子质量,通过与对照品或文献对照对其中10个特征成分进行了推测、确认。结论:采用高效液相色谱与质谱联用技术对续断指纹图谱中的特征峰进行结构确认,结束了续断色谱指纹盲分析的现状,可使其色谱指纹图谱的特征性更强,能更有效、全面的控制续断药材质量。
A high performance liquid chromatography(HPLC) method was developed for fingerprint of Dipsacus asper.Analysis were carried out on a Zorbax C-18 column by gradient elution using 0.1% phosphoric acid and acetonitrile as the mobile phases.The column was maintained at 25 ℃,the flow rate was 1 mL·min-1,and the detection wavelength was set at 205 nm.Asperosaponin VI was selected as reference compound,Seventeen common peaks were selected,and the fingerprint with good precision,stability and repeatability was successfully used to evaluate quality of 24 batches of crude extracts of D.asper.Chemical characteristics of D.asper was analyzed by DAD detection and HPLC-MS techniques with an ESI source.The quasi-molecular ions of compounds in both negative and positive modes were observed for molecule mass information of 33 compounds,and the potential structures of 10 characteristic components were identified by study on the mass spectra of compounds and comparing with reference data and some of standards.The results indicate the HPLC fingerprint of D.asper will show more characters through identification of component structures using an HPLC-ESI-MS method,and will control the quality of D.asper more effectively and reasonable.

关键词(KeyWords): 续断;指纹图谱;高效液相色谱;电喷雾质谱
Dipsacus asper;fingerprint;high performance liquid chromatography;electrospray mass spectrometry

Abstract:

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基金项目(Foundation): 国家自然科学基金项目(30973978)

作者(Author): 韦英杰;贾晓斌;樊宏伟;彭蕴茹;詹雯;
WEI Yingjie1,JIA Xiaobin1,FAN Hongwei2,PENG Yunru1,ZHAN Wen1(1.Key Laboratory of New Drug Delivery System of Chinese Meteria Medica,Jiangsu ProvincialAcademy of Chinese Medicine,Nanjing 210028,China;2.Lab of Clinical Pharmacology,Affiliated Nanjing First Hospital,Nanjing Medical University,Nanjing 210006,China)

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