滴眼液中13种常用抑菌剂含量测定的HPLC法建立及其在利巴韦林滴眼液测定中的应用  

A HPLC method for the determination of 13 common bacteriostatic agents in eye drops and its application in the determination of ribavirin eye drops

作　　者：罗建琴 冯雨薇 袁军 冯文 刘峰 钱广生[1] 无 LUO Jianqin;FENG Yuwei;YUAN Jun;FENG Wen;LIU Feng;QIAN Guangsheng;无(West China College of Pharmacy,Sichuan University,Chengdu 610041,China;Sichuan Institute of Drug Control,Chengdu 611730,China;NMPA Key Laboratory for Technical Research on Drug Products In Vitro and Vivo Correlation,Chengdu 611730,China)

机构地区：[1]四川大学华西药学院,四川成都610041 [2]四川省药品检验研究院,四川成都611730 [3]药物制剂体内外相关性技术研究重点实验室,四川成都611730

出　　处：《中国测试》2023年第4期73-79,共7页China Measurement & Test

摘　　要：建立同时测定滴眼液中13种常用抑菌剂含量的高效液相色谱法并应用于利巴韦林滴眼液中3种抑菌剂的含量测定。采用高效液相色谱法,使用YMC-Triart C18(4.6 mm×150 mm,3μm)色谱柱;以5 mmol·L^(-1)醋酸铵(含1%三乙胺,冰醋酸调pH5.0)为流动相A,乙腈为流动相B,梯度洗脱;流量1 mL·min^(-1);柱温35℃;检测波长214 nm;进样体积10μL。结果表明13种抑菌剂间分离度均达到要求,空白辅料不干扰抑菌剂测定;抑菌剂在各自线性范围内的线性关系良好;平均回收率在91.91%~102.2%范围内,RSD均小于2.0%;按拟定方法测定样品中硫柳汞钠含量为0.005~0.007 mg·mL^(-1),苯扎溴铵含量为0.0744~0.0935 mg·mL^(-1),羟苯乙酯含量为0.2309~0.356 mg·mL^(-1)。该方法灵敏、快速,专属性强,可同时实现滴眼液中多种抑菌剂的准确定性定量测定。A HPLC method for simultaneous determination of 13 common bacteriostatic agents in eye drops was established and applied to the determination of 3 bacteriostatic agents in ribavirin eye drops.High performance liquid chromatography was used with YMC triart C18(4.6 mm×150 mm,3μm)Chromatographic column;5 mmol·L^(-1) ammonium acetate(containing 1%triethylamine and adjusting pH 5.0 with glacial acetic acid)was used as mobile phase A and acetonitrile as mobile phase B;Flow rate was 1 mL·min^(-1);Column temperature was 35℃;Detection wavelength was 214 nm;Injection volume was 10μL.The separation degree of 13 bacteriostatic agents reached the requirements,and the blank excipients did not interfere with the determination of bacteriostatic agents.The linear relationship of bacteriostatic agents in their linear range was good.The average recoveries were in the range of 91.91%to 102.2%with RSDS less than 2.0%.According to the proposed method,the contents of sodium thiomersal,benzalammonium bromide and ethyl hydroxybenzoate were 0.005-0.007 mg·mL^(-1),0.0744-0.0935 mg·mL^(-1) and 0.2309-0.356 mg·mL^(-1) respectively.The method is sensitive,rapid and specific,and can be used for the accurate qualitative and quantitative determination of multiple bacteriostatic agents in eye drops.

关 键 词：利巴韦林 苯扎溴铵 硫柳汞钠 羟苯乙酯 高效液相色谱法 

分 类 号：TQ460.72[医药卫生—药物分析学] O657.72[化学工程—制药化工]