HPLC法测定联苯乙酸巴布剂中药物含量及其体外透皮性能的研究

目的:建立联苯乙酸巴布剂中联苯乙酸含量的HPLC测定方法,研究联苯乙酸巴布剂(LDH-Cata-plasm)的体外透皮释放性能,并与国外商品样品(J-Cataplasm)进行了比较。方法:高效液相色谱法,色谱柱:Wa-ters SunFireC18柱(150mm×4.6mm,5μm);流动相:甲醇-乙酸铵水溶液(60?40)(乙酸调节pH=3.6);流速:1.0mL/min,检测波长:254nm,进样量:10μL。用离体豚鼠皮肤作为透皮屏障,采用改进的Franz扩散池测定联苯乙酸巴布剂的体外透皮性能。结果:在1.26～20.16μg/mL浓度范围内,联苯乙酸浓度与峰面积之间呈良好线性关系,相关系数r=0.9999;定量限为0.05μg/mL;回收率为98.7%～100.0%。LDH-Cataplasm与J-Cataplasm的体外透皮方程均符合Higuchi方程(Q=kt1/2),且两者的体外透皮过程相似,各时间点的透皮速率无显著性差异。结论:该方法快速、简便,重复性好,可用于联苯乙酸巴布剂的含量测定及其体外透皮释放量的测定。

HPLC determination of 4-biphenylacetic acid content in felbinac cataplasm and study on in vitro skin permeation behavior of LDH-cataplasm

Objective：To establish a high performance Liquid chromatoraphy（HPLC） method for the determination of 4-biphenylacetic acid content in felbinac cataphlasm,and to study the in vitro skin permeation bevavior of LDH-cataplasm.Methods：High performance liquid chromatography was performed using a Waters Sunfire column（150mm×4.6mm,5μm）.The mobile phase was a mixture of methanol and 20mmol/L ammonium acetate（60 ：40） buffer solution adjusted with acetic acid to the pH of 3.6.The flow rate was 1.0 mL/min,the detection wavelength was 254nm,and the injection volume was 10μL.The in vitro skin permeation behavior of LDH-cataplasm was studied using the skin of a quinea pig as the transdermal barrier and a modified Franz cell for detection.The in vitro skin permeation behaviors of LDH-cataplasm and the foreign product J-cataplasm was compared.Results：A good linear relationship existed betwen the peak area and concentration（r=0.999,n=5） in the range of 1.26～20.16 μg/mL,the limit of quantification was 0.05 μg/mL,and the recovery was 98.7%～100.0%.The in vitro skin permeations of both LDH-cataplasm and J-calaplasm were in accordance with Highuchi equation,Q=kt^1/2,and the skin permeation processes were similar.There was no significant difference in the permeation rate at each time point.Conclusion：The method is rapid,simple and reproducible,and can be used for the determination of 4-biphenylacetic acid content in felbinac cataplasm and its released amount in the in vitro skin permeation.