咪唑斯汀缓释片稳定性分析法——HPLC法

The HPLC method developed for the stability study of mizolastine sustained-release tablet

目的 :建立咪唑斯汀缓释片的稳定性分析方法。方法 :采用高效液相色谱法。色谱柱为PhenomenexprodigyODS3 (2 5 0mm× 4 6mm ,5 μm) ;流动相 :甲醇 pH 4 0缓冲液 (7∶3) ;检测波长 2 80nm ;流速 1 0mL·min-1;外标法峰面积定量。结果 :咪唑斯汀保留时间约为 8 6min ,中间体、辅料、分解产物等对主药测定无干扰 ;咪唑斯汀浓度在 3～ 2 4 μg·mL-1范围内线性关系良好 ,回归方程为A =10 0 0 38 0 5C +6 5 5 6 ,r =0 99999;最低检出浓度为6 0ng·mL-1;日内、日间精密度 (RSD)分别为 0 39% (n =5 )和 0 5 6 % (n =5 ) ,重现性试验RSD =0 5 6 % (n =9) ;方法平均回收率为 99 4 7%～ 10 1 97% (n =5 ) ;模拟制剂平均回收率为 10 0 0 4 % (n =9)。结论 :该法灵敏、准确、专属性强 ,可用于咪唑斯汀片的稳定性研究。

Objective:To establish a HPLC method for the stability study of mizolastine sustained-release tablet.Methods:The chromatographic column was a Phenomenex prodigy ODS 3 column (250mm×4.6mm,5μm).The mobile phase,MeOH-pH 4.0 buffer solution (7∶3),was used at a rate of 1.0mL·min -1.The detection wavelength was 280nm and the external standard was adopted.Results:Under the condition of test,the retention time of mizolastine was about 8.6min.The intermediate,the pharmaceutical aids and the decomposition products could be well separated from mizolastine.The linear range was 3～24μg·mL -1 and the linear regression equation was A=100038.05 C+ 655.6 (r=0.99999).The lowest concentration of detection was 60ng·mL -1.RSD of intra-day and inter-day were 0.39% and 0.56% (n=5) respectively.RSD of repeatability was 0.56% (n= 9).The average recoveries of method were 99.47%～101.97% (n=5) and the average recovery of preparation simulating test was 100.04%(n=9).Conclusion:The method developed is accurate and reliable.It is very suitable for the stability study of mizolastine sustained-release tablet.