摘要
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.
作者
孙玉双
张锁庆
张文胜
杨梦德
刘远华
马亚微
贺娇
柳世萍
Sun Yu-shuang;Zhang Suo-qing;Zhang Wen-sheng;Yang Meng-de;Liu Yuan-hua;Ma Ya-wei;He Jiao;Liu Shi-ping(NCPC Hebei Pharma Co.,Shijiazhuang 052165)
出处
《中国抗生素杂志》
CAS
CSCD
2018年第12期1528-1532,共5页
Chinese Journal of Antibiotics