高效凝胶色谱法测定头孢呋辛酯及制剂中高分子杂质的含量

目的: 采用聚苯乙烯高效凝胶色谱法检查头孢呋辛酯中的高分子杂质。 方法: 色谱柱为MKF-GPC-100聚苯乙烯凝胶色谱柱(7.8 mm×100 mm,8 μm),流动相为水-甲醇(10∶90),流速为0.5 mL·min^-1,检测波长为278 nm;通过HPLC-ESI-MS²法鉴定高分子杂质峰,并对其结构进行推定。 结果: 头孢呋辛酯在0.5~1500 μg·mL^-1的浓度范围内,面积与浓度呈良好的线性关系(r=1.000);最小检出浓度为0.2 μg·mL^-1;高分子杂质与头孢呋辛酯峰能有效分离,并先于主峰流出,方法专属性良好;高分子杂质在溶液中不稳定,样品需要临用现配。 结论: 建立的方法快速准确,适用于酯溶性头孢呋辛酯及其制剂中高分子杂质的测定。

Objective: To determinate the high molecular mass impurities in cefuroxime axetil by polystyrene-based gel filtration chromatography. Method: A MKF-GPC-100 (7.8 mm×100 mm,8 μm) column was adopt with the mobile phase consisting of water-methanol(10∶90),at a flow rate of 0.5 mL·min^-1,and the detection wavelength was at 278 nm,to identify the impurities by HPLC-ESI-MS². Result: The calibration curves for cefuroxime axetil in the range of 0.5-1500 μg·mL^-1 was linear (r=1.000),the detection limit was 0.2 μg·mL^-1;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 solution,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 high molecular mass impurities in liposoluble drug cefuroxime axetil and it’s preparation.