HPLC-CDD法测定以碳酸钠为助溶剂的头孢类产品中碳酸钠的含量

HPLC-CDD determination of sodium carbonate(as a cosolvent) in cephalosporin products

目的建立高效液相-电导法(HPLC-CDD法)测定以碳酸钠为助溶剂的头孢类产品中碳酸钠的含量。方法以羧酸基键合硅胶为分析柱的填充剂(metrosep C47μm×100mm×4.0mm);流动相:(1.7mmol/L硝酸+0.7mmol/L吡啶二羧酸溶液)-乙腈(90:10);流速:1mL/min;柱温:35℃;进样量:20μL;检测器:非抑制型电导检测器。结果以注射用头孢他啶为例,钠离子在4.0～15.8μg/mL浓度范围内与其峰面积呈良好的线性关系,r=1.0000。高、中、低3种浓度的平均回收率为100.9%,RSD为0.5%。结论该方法简便、准确、灵敏度高,重现性好,可作为以碳酸钠为助溶剂的头孢类产品中碳酸钠的含量。

Objective To develop a method for the determination of sodium carbonate （as a cosolvent） in cephalosporin products using a HPLC method. Methods The chromatographic condition： the column was a silica gel with carboxylic groups particle （metrosep C4 7μm×100mm×4.0mm）, The mobile phase consisted of （1.Tmmol/ L nitric avid ＋0.7mmol/Ldipiconlinic avid）- acetonitrile （99： 1）, the detected was an electric conductivity detector, the flow rate was 1.0mL/min, the column temperature was 35℃, the sample size was 20μL. Results As ceftazidime for injection for example, the calibration curve was linear （r=l.0000）. in the range of 4.9-14.7μg/mL for sodium ion. The average recoveries was 100.9%（n=9）, and the average RSD was 0.5%. Conclusion The method is a accurate, simple, rapid, qualitative method with good reproducibility for quality contrct of sodium carbonate （as the complex solubilizer） in cephalosporin type antibiotics.