The Study Of Synthesis And Separation Effect Of Carboxyl Bonded Silica Stationary Phase For Separating Tanshinones

The Salvia miltiorrhiza Bge. is the Chinese traditional medicine for the Labiatae. It has high value in pharmacology activeness and is in wide use. The fat-soluble ingredients are extracted from it by ethyl alcohol, in which mainly are Cryptotanshinone, TanshinoneⅠand TanshinoneⅡA. In the industry, the traditional separation of Tanshinones mainly uses silica gel column chromatography. But silica gel has a disadvantage of irreversible absorption for the existence of silanol, which causes about 50% losses of Tanshinones, thus their recovery reduces greatly. It is determined the separation effect and irreversible adsorptive capacity of Tanshinones by study on the preparation, characterization, chromatographic performance of carboxyl bonded silica stationary phase and preliminary study on preparation column.First, a method based on HPLC to determine the fat-soluble components of Salvia miltiorrhiza is described. The content of Cryptotanshinone, TanshinoneⅠand TanshinoneⅡA is 3.33%, 3.19%, 17.40% respectively. This proposed method demonstrated good stability and reproducibility, and Cryptotanshinone, TanshinoneⅠand TanshinoneⅡA are stable in 48h at 10℃.Then, carboxyl bonded silica stationary phase is obtained by two steps. It is discussed the craft condition of preparation influence to its performance through the orthogonal experiment, which are its bonded amount and resolution of TanshinoneⅡA and TanshinoneⅠ. And It is investigated the influence of bonded amount and solvent polarity to their resolution and TanshinoneⅡA's peak area. The result is that this stationary phase is stable thermally at 160℃, but is unstable in water. Its bonded amount increases, then their resolution enhances and TanshinoneⅡA's peak area increases, is that the irreversible absorptive capacity reduces; Solvent polarity increases, then their resolution reduces and TanshinoneⅡA's peak area increases, is that the irreversible absorptive capacity reduces.Finally, it is studied preliminary the separation of Tanshinones on column chromatography. It is compared with the silica gel preparation column, the irreversible adsorptive capacity obviously reduces by carboxyl bonded silica stationary phase. The recovery of TanshinoneⅡA, TanshinoneⅠand Cryptotanshinone enhance 35.3%, 34.3%, 34.6% respectively. The purity of them enhance 2.3%, 2.4%, 0.2% respectively. So, it is feasible to increase Tanshinones recovery by carboxyl bonded silica stationary phase in preparation column.