高效液相色谱法测定头孢地尼及制剂中聚合物的含量

Determination of Polymer Content in Cefdinir and Preparations by HPLC

目的采用聚苯乙烯高效液相色谱法检查头孢地尼中聚合物的方法。方法色谱柱为聚苯乙烯凝胶为填料的TSKgel G2000SWxl(7.8 mm×300 mm 5um)色谱柱,流动相为0.1 mol/L,pH=7.0缓冲溶液-甲醇(95:5),流速为0.5 mL/min,检测波长285 nm,通过HPLC-ESI-MS法鉴定高分子杂质峰,并对其结构进行推定。结果头孢地尼在0.0002~1.5 mg/mL浓度范围内与峰面积呈良好线性关系(r=1.0000)最小检测浓度为0.2 ug/mL,聚合物杂质与头孢地尼能有效分离,并先于主峰流出,方法专属性良好,样品在溶液中不稳定,需临用新配。结论建立的方法快速准确。适用于头孢地尼及其聚合物的测定。

Objective To establish determination of polymer content in cefdinir by Polystyrene-High Performance Liquid Chromatography.Methods A TSKgel G2000SWxl(7.8í300mm 5um)column was adopt with the polystyrene gel column fil er mobile phase was 0.1mol/L pH=7.0 buf er solution-methanol(95:5),the flow rate was 0.5ml/min The detection wavelength was 285nm,to identify the impurities by HPLC-ESI-MS.Results The calibration curves for cefdinir in the range of 0.0002mg/ml^1.5mg/ml was linear(r=1.0000)the detection limit was 0.2ug/ml,the peaks before cefuroxime axetil in the chromatogram were high molecular mass impurities,the resolution between cefuroxime axetil and high molecular mass impurities was good.The high molecular mass impurities is instable in so-lution,and the test solution should be prepared immediately before use.Conclusion The established method is fast for analysis and good for precision,it's suitable for determinate the polymer in cefdinir and it's preparation.