摘要
目的：建立HPLC梯度洗脱法同时测定盐酸头孢他美酯中的有关物质和聚合物。方法：采用Thermo AcclaimTM120 C18色谱柱（250 mm×4.6 mm,5μm）,流动相A为乙腈-甲醇-水-磷酸盐缓冲液（180︰47.5︰750︰67.5）,流动相B为乙腈-甲醇-水-磷酸盐缓冲液（540︰142.5︰250︰22.5）,梯度洗脱（0 min,0%B;2 min,0%B;30 min,100%B;45 min,100%B;46min,0%B;55 min,0%B）,流速为1.0 m L·min^-1,检测波长为233 nm。结果：盐酸头孢他美酯与中间体、分解产物完全分离。杂质头孢他美酸、AE活性酯和7-氨基-3-去乙酰氧基头孢烷酸（7-ADCA）的回收率分别为97.8%、98.3%和104.4%,重复性RSD为2.8%,定量限为0.04～0.21μg·mL^-1。各有关物质测定结果,头孢他美酸为1.0%～1.6%,异构体1为0.2%～0.9%、异构体2为0.1%～0.2%、二聚物1为0.1%～0.3%、二聚物2为0.2%～0.8%。结论：建立的方法经方法学验证可用于本品的质量控制。
Objective： To develop an HPLC-gradient elution method for simultaneous determination of related substances and polymers in cefetamet pivoxil hydrochloride. Methods： The column was Thermo AcclaimTM120 C18（ 250 mm × 4. 6 mm,5 μm）. The mobile phase consisted of acetonitrile-methanol-water-phosphate buffer（ 180︰47. 5︰750︰67. 5）（ A） and acetonitrile-methanol-water-phosphate buffer（ 540︰142. 5︰250︰22. 5）（ B）with gradient elution program（ 0 min,0% B; 2 min,0% B; 30 min,100% B; 45 min,100% B; 46 min,0% B; 55 min,0% B）. The flow rate was 1. 0 m L·min^-1,and the detection wavelength was 233 nm. Results： Good separation of cefetamet pivoxil from intermediates and degradation products was achieved. The recoveries of impurities cefetamet acid,AE active ester and 7-aminodesacetoxycephalosporanic acid（ 7-ADCA） were 97. 8%,98. 3% and104. 4%. The RSD of repeatability was 2. 8%. The quantitation limit was 0. 04-0. 21 μg·mL^-1. The contents of cefetamet acid,isomer 1,isomer 2,dimer 1 and dimer 2 were 1. 0%-1. 6%,0. 2%-0. 9%,0. 1%-0. 2%,0. 1%-0. 3% and 0. 2%-0. 8%. Conclusion： The method meets the requirement of methodology validation,and can be used for quality control of cefetamet pivoxil hydrochloride.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2015年第2期295-300,共6页
Chinese Journal of Pharmaceutical Analysis
基金
浙江省公益性技术应用研究计划分析测试科技计划项目计划编号2013C37057
