盐酸头孢唑兰高分子聚合物的测定
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摘要
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 ~ 120 μm). 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 flow rate was 1. 0 ml / min,the detection wavelength was 254 nm and the injection volume was 100 μl. The concentration of polymers was quantified by external standard method of cefatriaxone with a corrected factor( cefozopran: cefatriaxone = 1. 19∶ 1). Results The cefozopran showed good linearity with peak area of high molecular polymers in cefozopran hydrochloride 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 molecular polymers in cefatriaxone in the range of 24. 56 μg / ml ~ 245. 6 μg / ml( r = 0. 9997). The limit of detection was 0. 025 μg and the limit of quantitation was 0. 083 μg. Conclusion The method can be used to separate the high molecular polymers from cefozopran preferably and it was suitable for high molecular polymers detection in cefozopran hydrochloride for injection.
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 ~ 120 μm). 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 flow rate was 1. 0 ml / min,the detection wavelength was 254 nm and the injection volume was 100 μl. The concentration of polymers was quantified by external standard method of cefatriaxone with a corrected factor( cefozopran: cefatriaxone = 1. 19∶ 1). Results The cefozopran showed good linearity with peak area of high molecular polymers in cefozopran hydrochloride 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 molecular polymers in cefatriaxone in the range of 24. 56 μg / ml ~ 245. 6 μg / ml( r = 0. 9997). The limit of detection was 0. 025 μg and the limit of quantitation was 0. 083 μg. Conclusion The method can be used to separate the high molecular polymers from cefozopran preferably and it was suitable for high molecular polymers detection in cefozopran hydrochloride for injection.
引文
[1]王诗鸿.第四代头孢菌素头孢唑兰[J].中国新药杂志,2006,15(4):312.
[2]蒋锦,刘秉全,郭慧元.第四代头孢菌素盐酸头孢唑兰[J].国外医药抗生素分册,2006,27(2):61.
[3]蔡姗英.胡昌勤.β-内酰胺类抗生素中高分子聚合物的分离分析方法研究进展[J].广东药学院学报,2002,18(2):138-142.
[4]中华人民共和国国家药典委员会.中华人民共和国:2010年二部[M].北京:中国医药科技出版社,2010.
[5]霍秀敏.β-内酰胺类抗生索高分子杂质质量控制研究中需注意的问题[J].药品评价,2005,2(5):324-326.
[6]蔡姗英,胡昌勤,冯芳.β-内酰胺抗生素在Superdex peptide凝胶过滤色谱柱上的色谱行为[J].中国抗生素杂志,2002,27(3):157-161,192.
[2]蒋锦,刘秉全,郭慧元.第四代头孢菌素盐酸头孢唑兰[J].国外医药抗生素分册,2006,27(2):61.
[3]蔡姗英.胡昌勤.β-内酰胺类抗生素中高分子聚合物的分离分析方法研究进展[J].广东药学院学报,2002,18(2):138-142.
[4]中华人民共和国国家药典委员会.中华人民共和国:2010年二部[M].北京:中国医药科技出版社,2010.
[5]霍秀敏.β-内酰胺类抗生索高分子杂质质量控制研究中需注意的问题[J].药品评价,2005,2(5):324-326.
[6]蔡姗英,胡昌勤,冯芳.β-内酰胺抗生素在Superdex peptide凝胶过滤色谱柱上的色谱行为[J].中国抗生素杂志,2002,27(3):157-161,192.