盐酸头孢唑兰高分子聚合物的测定

Determination of high molecular polymers in cefozopran hydrochloride

目的建立难溶于水药物盐酸头孢唑兰中高分子聚合物的测定方法。方法采用分子排阻色谱法,葡聚糖凝胶G-10(40μm^120μm)为填充剂的玻璃柱(1.0 cm×30 cm),分别以pH7.0的0.05 mol/L磷酸盐缓冲液和水为流动相A和流动相B;流速1.0 ml/min,检测波长为254 nm,进样量为100μl。以头孢曲松替代不完全聚合的头孢唑兰作为对照,加校正因子外标法定量(头孢唑兰:头孢曲松=1.19∶1)。结果头孢唑兰浓度在2.00 mg/ml^20.0 mg/ml范围内与盐酸头孢唑兰中高分子聚合物峰面积呈良好的线性关系(r=0.9999),头孢曲松对照品浓度在24.56μg/ml^245.6μg/ml范围内与头孢曲松中高分子聚合物峰面积呈良好的线性关系(r=0.9997)。检测限为0.025μg,定量限为0.083μg。结论经验证该方法能够较好地分离头孢唑兰和高聚物,可用于注射用盐酸头孢唑兰的高分子聚合物的检测。

Objective To establish a method for determination of high molecular polymers level in cefozopran hydrochloride. Methods Chromatography analysis was performed on a glass column （ 1.0 cm × 30 cm）filled with sephadex G - 10 （40 μm- 120μm）. The mobile phase was consisted of 0.05 mol/L phosphate buffer（pH = 7.0） as mobile phase A and water as mobile phase B. The ilow rate was 1.0 ml/min, the detection wavelength was 254 nm and the injection volume was 100 p^l. The con- centration of polymers was quantified by external standard method of cefatriaxone with a corrected factor （ cefozopran： cefatriax- one = 1.19：1 ）. Results The cefozopran showed good linearity with peak area of high molecular polymers in cefozopran＇hydro- chloride in the range of 2.00 mg/ml-20.0 mg/ml （r =0. 9999）. And the cefatriaxone was linear with peak area of high mo- lecular polymers in cefatriaxone in the range of 24. 56μg/ml - 245.6 μg/ml （ r = 0. 9997 ）. The limit of detection was 0. 025μg and the limit of quantitation was 0. 083μg. Conclusion The method can be used to separate the high molecular pol- ymers from cefozopran preferably and it was suitable for high molecular polymers detection in cefozopran hydrochloride for injec- tion. Key Words： Cefozopran hydrochloride; High molecular polymers; Molecular exclusion chromatography