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

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+5mmol.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。

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 offline 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.