注射用氯唑西林钠中氯唑西林噻唑酸的分离及含量检测  

Separation and assay of cloxacilloic acid in cloxacillin sodium for injection samples

作　　者：杜康丽 郭鹏琦 傅强[2] 

机构地区：[1]天津市环湖医院药剂科,天津300060 [2]西安交通大学药学院,陕西西安710061

出　　处：《中国医院药学杂志》2017年第22期2226-2230,共5页Chinese Journal of Hospital Pharmacy

基　　金：国家自然科学基金项目(编号:81173024)

摘　　要：目的:实现注射用氯唑西林钠中氯唑西林噻唑酸的分离及含量检测。方法:采用分子印迹-溶胶凝胶技术,以氯唑西林噻唑酸为模板,在活化硅胶表面制备具有特异性的分子印迹聚合物,并对合成条件进行优化。采用扫描电镜对聚合物进行形貌表征。将聚合物作为固相萃取填料,结合高效液相色谱法对氯唑西林钠中氯唑西林噻唑酸进行分离及含量检测。结果:当模板分子、功能单体和交联剂的摩尔比为1∶4∶28,溶剂为3 mL,催化剂为300μL,反应温度为30℃时,聚合物的吸附量和印迹因子最佳。扫描电镜结果显示聚合物已成功接枝到硅胶表面。氯唑西林噻唑酸分子印迹聚合物和固相萃取相结合的方法,经方法学验证,在0.5~50 mg·g^(-1)范围内呈现良好的线性关系(r=0.996 2),检测限为0.07 mg·g^(-1)。结论:该方法的专属性、准确度和精密度均良好,能够实现氯唑西林钠中微量杂质氯唑西林噻唑酸的分离及含量检测。OBJECTIVE To separate and detect cloxacilloie acid in eloxacillin sodium for injection samples. METHODS The molecularly imprinted polymers were prepared using cloxacilloic acid as template on the surface of silica gels by the sol-gel process, and the synthesis conditions were optimized. The surface morphology was analyzed by scanning electron microscope. The polymers were used as solid phase extraction sorhents coupled with HPLC for the analysis of cloxacilloic acid in the clox- acillin sodium samples. RF^ULTS When the molar ratio of template, functional monomer and cross-linker was 1 ： 4 ： 28, the contents of solvent and catalyst were 3 mL and 300μL, respectively, and when the temperature was 30℃, the adsorption ca- pacity and imprinting factor reached the optimun values. The scanning electron microscope indicated deposition of the polymers over the surface of the silica gels. The linearity range of this method was 0. 5 - 50 mg.g^-1 （r= 0. 996 2） and the limit of detec- tion was 0. 07 mg·g^-1. CONCLUSION This method has good specificity, accuracy and precision, and can separate and detect the cloxacilloic acid in the cloxacillin sodium samples.

关 键 词：致敏性杂质 氯唑西林 分子印迹-溶胶凝胶技术 固相萃取技术 高效液相色谱法 

分 类 号：R927.2[医药卫生—药学]