丹参酮色谱分离中羧基键合固定相作用研究

Study on the carboxyl bonded silica stationary phase for chromatographic separation of tanshinones

目的:合成羧基键合硅胶固定相并将其用于分离丹参酮,以期减小对丹参酮的不可逆吸附。方法:以己二酸为原料合成了羧基键合硅胶固定相,利用红外光谱和热重分析对其进行表征。以石油醚(60～90℃)-乙酸乙酯(85:15)为流动相,用高效液相色谱对合成固定相在分离丹参酮的吸附能力和分离效果进行了评价,并与硅胶进行比较。结果:丹参酮ⅡA和丹参酮Ⅰ在羧基键合相的分离度由0.81提高到1.36;不可逆吸附比较硅胶降低了约37%。结论:羧基键合硅胶固定相可用于分离丹参酮以减小对其不可逆吸附。

Objective： Synthesize carboxyl bonded silica stationary phase for separation of tanshinones, reducing the irreversible adsorption of tanshinones was suggested. Method： With adipic acid bonded on silica gel by using two step responses, carboxyl bonded silica stationary phase was obtained. Characterization of prepared packing was carried out with fourier transform infrared （FTIR） spectroscopy and thermogravimetric analysis. Chromatographic evaluations were carried out with tanshinones using petroleum ether （60 -90 ℃ ） -ethyl acetate （85：15 ,v/v） as mobile phase. Result： The resolution of tanshinone Ⅱ A and tanshinone I is up to 1.36 on the column packed carboxyl bonded silica stationary phase, and compared with silica gel, the irreversible adsorptive capacity of carboxyl bonded silica stationary phase reduces about 37%. Conclusion：Carboxyl bonded silica stationary phase can be used in separating tanshinones to reduce its irreversible adsorption.