HPLC同时测定双氯芬酸钠滴眼液中3种抑菌剂的含量

Simultaneous Determination of 3 Bacterial Inhibitors in Diclofenac Sodium Eye Drops by HPLC

关键词:  抑菌剂  双氯芬酸钠滴眼液  羟苯乙酯  硫柳汞  苯扎氯铵  含量测定

Key words:  bacterial inhibitor  diclofenac sodium eye drops  ethyl hydroxybenzoate  thiomersal  benzalkonium chloride  content determination

摘要:

目的 建立HPLC同时测定双氯芬酸钠滴眼液中羟苯乙酯、硫柳汞和苯扎氯铵含量的方法。方法 用十八烷基键合硅胶为填充剂，以1%三乙胺溶液（磷酸调节pH值至3.0）为流动相A，以甲醇为流动相B，进行梯度洗脱；流速1.0 mL·min^-1，柱温40℃，检测波长254 nm。结果 羟苯乙酯在20.58~205.8 μg·mL^-1、硫柳汞在8.242~82.42 μg·mL^-1、苯扎氯铵n-C₁₂H₂₅取代物在12.88~128.8 μg·mL^-1、苯扎氯铵n-C₁₄H₂₉取代物在6.624~66.24 μg·mL^-1内线性良好（r≥0.999 8），平均回收率为99.3%~102.5%（n=9）。结论 该方法简单、准确、重复性好，可用于控制双氯芬酸钠滴眼液中羟苯乙酯、硫柳汞和苯扎氯铵的含量。

Abstract:

BJECTIVE To establish a method for the simultaneous determination of ethyl hydroxybenzoate, thiomersal and benzalkonium chloride in diclofenac sodium eye drops by HPLC. METHODS The C₁₈ column was used as analytical column, with 1% triethylamine solution(phosphoric acid adjusted pH to 3.0) as mobile phase A, and methanol as mobile phase B with gradient elution. The column temperature was kept at 40℃. The flow rate was 1.0 mL·min^-1. The detection wavelength was set at 254 nm. RESULTS Between 20.58-205.8 μg·mL^-1(ethyl hydroxybenzoate), 8.424-82.42 μg·mL^-1(thiomersal), 12.88-128.8 μg·mL^-1(benzalkonium chloride n-C₁₂H₂₅), 6.624-66.24 μg·mL^-1(benzalkonium chloride n-C₁₄H₂₉), their linearities were good, with their recoveries were between 99.3%-102.5%(n=9). CONCLUSION The method is simple, accurate and reproducible. It can be used to control the content of ethyl hydroxybenzoate, thiomersal and benzalkonium chloride in diclofenac sodium eye drops.