亲水作用色谱法测定表阿霉素及其杂质

建立了一种以亲水作用色谱分离测定表阿霉素的新方法。采用硅胶色谱柱及高极性有机溶剂水相缓冲溶液流动相。对流动相的pH、缓冲溶液的浓度及流速进行了优化,确定了以乙腈甲酸钠缓冲溶液(pH2.9)(90∶10,V/V)作为流动相的最佳条件。对优化的分离条件进行系统适应性实验,结果表明表阿霉素与有关杂质之间的分离度和拖尾因子均达到药典要求。该法具有良好的线性(相关系数0.9971～0.9991)和重复性(峰面积RSD<1.0%),方法简便实用,用于实际样品分析,结果满意。

Determination of Epirubicin and Its Impurities in Pharmaceutical by Hydrophilic Interaction Chromatography

A novel method for the determination of epirubicin by hydrophilic interaction chromatography (HILIC) using high purity silica column with highly polar organic-aqueous buffer as mobile phase has been developed. The buffer pH and concentration in the mobile phase as well as the flow rate have been optimized. The optimal mobile phase is 90% (V/V) acetonitrile in 40 mmol/L formate buffer (pH 2.9). The flow rate was 1.0 mL/min. The system suitability has been tested under the optimal chromatographic condition, and the results show that the resolutions between the adjacent components and the asymmetry factors of the solutes meet the pharmacopoeia requirements. The proposed method has good linearity (r=0.9971~0.9991) and reproducibility (RSD<1.0% for the peak area). It has been proved simple and convenient, and applied in the determination of epirubicin and its impurities in epirubicin raw product with satisfactory results.