大黄中鞣质成分的分离与液相色谱/质谱联用分析

Separation of Tannins in Rhubarb and Its Analysis by High Performance Liquid Chromatography-Mass Spectrometry

研究了大黄中鞣质类成分的提取、分离与分析方法。优化了大黄原药材中鞣质类物质的提取方法;建立了大黄鞣质类成分的梯度洗脱反相高效液相色谱(HPLC)分析方法,使鞣质类成分得到了良好的分离;采用液相色谱 质谱(LC MS)对大黄中主要的鞣质类化合物进行了结构分析,并总结了一部分鞣质类化合物在高效液相色谱 电喷雾质谱(HPLC ESI MS)谱图上的裂解规律。

In order to investigate the pharmaceutical actions of rhubarb, a method for extracting, separating and analyzing the tannin components in rhubarb was studied. At first, a procedure for the group separation of tannins from the water-ethanol extract of rhubarb was established based on the formation of tannins-caffein precipitation. Then, a high performance liquid chromatographic (HPLC) method for the analysis of tannins in rhubarb was developed. This HPLC method is based on a reversed-phase C_(18) column and polar mobile-phase such as water and methanol with gradient elution, and the tannins can be well separated. Finally, the (identification) of the tannin components in rhubarb was carried out by high performance liquid chromatography-mass spectrometry (HPLC-MS). The structures of the main tannin components (gallic acid, catechin, the dimer, trimer, tetramer and pentamer of catechin) in rhubarb are suggested. The fragmentation laws of the tannin components are summarized. In comparing with previous methods, it is simple and without the interference of co-existed compounds.