十八碳酰基高聚物型色谱填料的制备与用于七叶皂甙钠分离的研究

Preparation of C18-Acyl Polymer-based Chromatography Packing and It's Application in Sodium Aescinate Separation

将硬脂酸酰氯化后,与粒径单分散的苯乙烯-二乙烯基苯微球进行Friedel-Crafts酰基化反应得到以聚苯乙烯为基质的十八碳酰基麦科菲高聚物型色谱填料(MKF-PS-C18),用红外光谱、担载量和酰基化前后分离性能的比较对填料进行了表征。比较了MKF-PS-C18基质与硅胶基质在有机相和水梯度条件下的色谱柱压性能。讨论了流动相中有机溶剂的种类和浓度、离子对试剂种类和固定相的担载量等色谱条件对MKF-PS-C18填料分离七叶皂甙钠的影响。结果表明:MKF-PS-C18基质具有与硅胶基质相同的优越柱压性能。MKF-PS-C18色谱柱在优化的色谱条件(流动相:A为0.1%(体积分数)三氟乙酸(TFA),B为乙腈;温度:25℃;流速:1.0 mL/min;紫外检测:220 nm)下,对七叶皂甙钠中4种主要活性成分具有较好的分离性能。

MKF polystyrene-divinylbenzene（PS-DVB）C18（MKF-PS-C18） reversed phase stationary was prepared by treating corresponding microspheres of uniform diameter with stearyl chloride and characterized with infrared spectra,loading capacity and separation performance.The effects of organic solvents and their concentrations,ion pairing reagents and loading capacity of solid phase on the separation of sodium aescinate had been evaluated.The results showed that MKF-PS-C18 has the same column back pressure as silica gel.The four substances in sodium aescinate were separated on a MKF-PS-C18 column with mobile phases（A） water containing 0.1%（by volume）TFA and（B） acetonitrile at temperature of 25 ℃ and a flow rate of 1.0 mL/min and then detected at the wavelength of 220 nm.The results were satisfactory.