TSK凝胶色谱系统测定头孢丙烯干混悬剂中的高分子杂质

Determination of polymers in cefprozil for suspension by the TSK-GEL chromatography system

目的建立针对头孢丙烯干混悬剂中高分子杂质的检测方法。方法采用HPLC法,色谱柱为TSK-GEL G2500PWXL(7.8mm×30mm, 7μm),以0.1mol/L pH6.8磷酸盐缓冲液为流动相,流速0.8mL/min,波长254nm,进样体积为20μL。结果高分子杂质峰与头孢丙烯(Z)异构体峰能有效分离,辅料不产生干扰,方法专属性良好;头孢丙烯溶液在4.6944～93.8880μg/mL浓度范围内线性关系良好,线性回归方程为y=24226.5x-19.3(r=1.0000);检测限为0.183μg/mL;定量限为0.549μg/mL;方法精密度良好(RSD=0.9%),中间精密度良好(RSD=0.6%);头孢丙烯干混悬剂中高分子杂质均低于1.5%。结论该方法操作简便、检测灵敏度高、方法重现性好,适用于头孢丙烯干混悬剂高分子杂质的检测。

Objective To establish a method for the determination of high molecular polymers in cefprozil for suspension by the TSK-GEL chromatography system.Methods The detection was conducted under the following conditions using high pressure liquid chromatography(HPLC):Chromatographic column was TSK-GEL G2500 PWXL(7.8mm×30mm,7μm);the mobile phase was 0.1mol/L pH6.8 phosphate buffer;the flow rate was 0.8mL/min; the detection wavelength was 254nm and the injection volume was 20gL.Results High molecular polymers was separated completely from cefprozil (Z)-isomer.The accessories made no interference.It has good specificity.Within the range of 4.6944-93.8880μg/mL of the cefprozil solution,the calibration curve was liner.The regression equation was y=24226.5x-19.3(r=1.0000).For cefprozil,the detection limit was 0.183μg/mL,and the quantitation limit was 0.549μg/mL.The repetitiveness was good (RSD=0.9%),and the intermediate precision was good (RSD=0.6%).The content of polymers in cefprozil for suspension is less than 1.5%.Conclusion The method has simple operations, high detection sensitivity,and good reproducibility,For the determination of the high molecular polymers in cefprozil for suspension,the method was suitable.