高效液相色谱法测定口腔护理双氯芬酸含漱液中双氯芬酸的含量

Determination of diclofenac content in collutorium by HPLC

目的建立高效液相色谱法(HPLC)测定双氯芬酸含漱液中双氯芬酸的含量方法。方法采用Zorbax SB-C18(4.6 mm×150 mm,5μm)色谱柱,流动相为A(0.1%甲酸),B(乙腈);0 min^6 min,30%~50%B;6 min^12 min,50%~70%B。流速为1.0 ml/min,检测波长为278 nm,柱温为30℃,进样量为10μl。结果双氯芬酸的浓度为0.1 g/ml^50 g/ml时,与峰面积的线性关系良好(r=0.997 6),最低检出限为0.1 g/ml。精密度RSD为0.24%,稳定性RSD为0.89%,平均回收率为98.32%。结论该法操作简便、快速,可用于双氯芬酸含漱液的质量控制。

Objective To establish a high performance liquid chromatography（HPLC） method for the determination of diclofenac in collutorium.Methods Zorbax SB-C18（4.6 mm×150 mm,5 μm） column was adopted for separation.A gradient elution programme was conducted for chromatographic separation with mobile phase A（0.1% formic acid in water） and mobile phase B（acetonitrile） as follows：0 min-6 min（30%-50% B）,6 min-12 min（50%-70% B）.The flow rate was1.0 ml/min.The detection wavelength was 278 nm and the column temperature was 30℃.A typical injection volume was10 μl.Results Good linearity was obtained when the concentration of diclofenac was within 0.1 μg/ml-50 μg/ml（r=0.997 6）.The detection limit was 0.1 μg/ml.The precision（RSD） was 0.24%.The result of stability（RSD） was 0.89%.The average recovery was 98.32%.Conclusion The method is simple and accurate,so it is suitable for the determination of diclofenac in collutorium.