高效液相色谱-电喷雾飞行时间质谱分析丹参中的丹参酮类化合物

Analysis of Diterpene Quinones in Danshen ( Salvia Miltiorrhiza Bunge ) by HPLC-ESI/TOFMS

  • 摘要: 采用高效液相色谱-电喷雾飞行时间质谱(HPLC-ESI/TOFMS)联用技术,研究4种丹参酮的分子结构与裂解规律间的关系,并对丹参酮中的脂溶性成分进行鉴定。采用反相C18色谱柱,以甲醇-0.1%乙酸+5 mmol•L-1 乙酸铵溶液为流动相,二元等度洗脱。通过与电喷雾飞行时间质谱联用,获得丹参中脂溶性成分的精确相对分子质量和分子式,采用质谱碰撞诱导解离技术获得各化合物碎片的裂解信息,并对丹参中的16种丹参酮类化合物进行了初步鉴定。研究结果表明,高效液相色谱电喷雾飞行时间质谱联用技术能够简便、快速、有效地鉴别丹参中的丹参酮类化合物。

     

    Abstract: The diterpene quinone components in lipid soluble fractions of Danshen were studied by HPLC-ESI/TOFMS. The lipid solubles were extracted with a mixture of chloroform and methanol (1∶4, V/V). The extract was dried by a gentle stream of nitrogen, and the residue was diluted in methanol for analysis. HPLC was performed on a reversed-phase C18 column using isocratic elution with a mixture of methanol and water with the addition of 0.1% acetic acid and 5 mmol•L-1 ammonium acetate. Accurate molecular weights of individual tanshinones were determined through ESI-TOF/MS on-line detection. The molecular formula and TOFMS fragmentation behavior of each compound were obtained through off-line analysis under different collision induced dissociation (CID) energies. Combining literature information with the observed data, 16 tanshinones in lipid-soluble fractions of Danshen were tentatively identified in a run. The method demonstrates high potential as a rapid and effective method for the preliminary structural screening and speciation of bioactive tanshinone components in Danshen or other herbal extracts.

     

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