摘要
目的:建立同时测定氟比洛芬酯注射液中溶血磷脂酰胆碱(LPC)和溶血磷脂酰乙醇胺(LPE)含量的方法。方法:采用HPLC法,蒸发光散射检测器,色谱柱为Zorbax RX-SIL(250 mm×4.6 mm,5μm)柱,以流动相A:甲醇-水-冰醋酸-三乙胺(85∶15∶0.45∶0.05),流动相B:正己烷-异丙醇-流动相A(20∶48∶22)梯度洗脱,流速为1.0 ml·min^-1,柱温为40℃,漂移管温度为75℃,雾化气流速为1.5 L·min^-1,进样量为20μl。结果:LPC和LPE分别在82.72~517.03μg·ml-1(r=0.9999)、19.19~119.93μg·ml-1(r=0.9990)范围内,浓度的对数值与其峰面积的对数值呈现良好线性关系;LPC和LPE的回收率分别为95.44%(RSD=1.10%,n=9),97.54%(RSD=1.52%,n=9)。36批制剂中均检出LPC和LPE,并且溶血磷脂含量随时间和温度增加而增加。结论:建议贮藏条件为25℃以下密闭储存,不可冷冻,有效期为12个月。该方法操作简便,可用于氟比洛芬酯注射液中有害杂质溶血磷脂的含量测定。
Objective:To establish a method for the simultaneous determination of lysophophatidyl choline(LPC)and lysophosphatidyl ethanolamine(LPE)in flurbiprofen axetil injection by HPLC-ELSD.Methods:A Zorbax RX-SIL(250 mm×4.6 mm,5μm)column was used with the mobile phase A consisting of methanol-water-glacial acetic acid-triethylamine(85∶15∶0.45∶0.05)and the mobile phase B consisting of hexane-isopropanol-mobile phase A(20∶48∶22)with gradient elution.The flow rate was 1.0 ml·min-1 and the column temperature was 40℃.The drift tube temperature was 75℃and the atomization gas flow rate was 1.5 L·min-1.The injection volume was 20μl.Results:LPC and LPE had a good linearity within the range of 82.72-517.03μg·ml-1(r=0.9999)and19.19-119.93μg·ml-1(r=0.9990),respectively.The logarithm values of injection concentration and peak areas showed good linear relationship.The recoveries of LPC and LPE were 95.44%(RSD=1.10%,n=9)and 97.54%(RSD=1.52%,n=9),respectively.LPC and LPE were both detected out in 36 batches of flurbiprofen axetil injection and the contents increased with time and temperature.Conclusion:The injection should be stored in a tightly closed container under 25℃in dark place,and can’t be frozen.Under the above storage conditions,the shelf-time of the injection is 12 months.The method is easy to operate,which is suitable for the determination of detrimental impurities in flurbiprofen axetil injection.
作者
陈蓉
苏静华
郝刚
Chen Rong;Su Jinghua;Hao Gang(Suzhou Institute for Drug Control,Jiangsu Suzhou 215104,China)
出处
《中国药师》
CAS
2020年第1期151-154,共4页
China Pharmacist
基金
苏州市科技计划项目(编号:SYS201781)
