高效分子排阻色谱法检测头孢泊肟酯中的聚合物及其结构推测  

Determination of Polymers in Cefpodoxime Proxetil by High Performance Size Exclusion Chromatography and Its Structure Postulation

作　　者：蒋惠源 钱忠义 孙青 JIANG Huiyuan;QIAN Zhongyi;SUN Qing(Taizhou Institute for Drug Control,Taizhou 225300;Management Committee of Taizhou Medical New&Hi-tech Industrial Development Zone,Taizhou 225300)

机构地区：[1]泰州市药品检验院,江苏泰州225300 [2]泰州医药高新技术产业园区管理委员会,江苏泰州225300

出　　处：《中国医药工业杂志》2020年第8期1048-1055,共8页Chinese Journal of Pharmaceuticals

摘　　要：本研究采用高效分子排阻色谱法测定头孢泊肟酯中聚合物的含量,并用液相色谱-串联质谱法对其中一个二聚物的结构进行推测。采用TSKgel G2000SWXL凝胶色谱柱,流动相为0.005 mol/L乙酸铵溶液(用氨水调至pH 7.0)∶甲醇(70∶30)。结果显示,头孢泊肟酯主峰前的杂质峰为聚合物,且能与主峰有效分离,方法专属性良好;主峰的线性范围为0.5~1200μg/ml,检测限为0.25μg/ml,定量限为0.75μg/ml,精密度良好。聚合物峰面积在头孢泊肟酯0.2~1.5 mg/ml浓度内呈线性,重复性良好,所建方法专属性强、耐用性好,灵敏度高,适用于头孢泊肟酯中聚合物的测定。In this study,a high performance size exclusion chromatography method was established to determine the polymer content in cefpodoxime proxetil,and the structure of one of the dimers was postulated by liquid chromatography-mass spectrometry.A TSKgel G2000SWXL gel chromatography column was used,and the mobile phase was 0.005 mol/L ammonium acetate solution(adjusted to pH 7.0 with ammonia solution)∶methanol(70∶30).The results showed that the impurity peaks before the main peak of cefpodoxime proxetil were the dimers,and they could be separated effectively from the main peak,which indicated that the method had good specificity.The linear range of the main drug was 0.5-1200μg/ml.The detection limit was 0.25μg/ml,and the limit of quantification was 0.75μg/ml,so that the method had good precision.The peak area of the polymer was linear in the concentration range of 0.2-1.5 mg/ml of cefpodoxime proxetil with good repeatability.The method has strong specificity,good durability and high sensitivity,which is suitable for the determination of polymers in cefpodoxime proxetil.

关 键 词：高效分子排阻色谱法 头孢泊肟酯 聚合物 脂溶性抗菌药 液相色谱-串联质谱法 

分 类 号：R927[医药卫生—药学] O657.7[理学—分析化学]