利用高效液相層析法分析Ketoprofen製劑及其分析法之驗證

A Stability-indicating Assay HPLC Method of Ketoprofen

許淑纓(Shu-Ying Hsu) ； 邵清益(Ching-Yih Shaw) ； 張柏林(Ber-Lin Chang)

《藥物食品分析》 3卷4期 (1995/12) Pp. 275-285

摘要

本報告敘述一種快速、靈敏，可供作安定性指標之Ketoprofen及其製劑中主成分、不純物及其變質產物之高效液相層析法。其分析系統之適宜性、專一性、線性、精密到定性、臨界濃度、線性範圍經適宜之統計解析均加以確認。利用Zorbax ODS C18 4.6×150 mm Column為國定相，0.05M KH2PO4/CH3CN (55:45, v/v)為移動相，流速為1.2 ml/min，檢測為UV 265 nm，並以Flurbiprofen為內部標準品，可分離Ketoprofen及其主要之酸、鹼水解物及光分解物，定量之直線濃度範圍為1.25 mcg/ml~20 mcg/ml，5 mcg/ml濃度（常用定量濃度）之同日內變動RSD及異日間變動RSD均小於10^(-2)%，本分析方法確為可應用於Ketoprofen原料藥之定性、定量、純度實驗及含該成分製劑之安定性定量分析。

並列摘要

The present official method for the assay and analysis of the ketoprofen related substances as described in the British Pharmacopeia is redox titration and thin layer chromatography. The assay method of ketoprofen preparation in the United States Pharmacopeia is an UV/VIS method. The National Laboratories of Foods and Drugs, ROC, require a rapid, sensitive and precise method for the analysis of large numbers of samples including those for ketoprofen. Since the existing official methods for ketoprofen are not all specific for ketoprofen, a specific HPLC method is then desirable. This report presents such an approach. The HPLC system consisted of a Zorbax ODS C18 (4.6×150mm) and a mobile phase of aqueous KH2PO4 with glacial acetic acid in CH3CN (55/45, v/v) at pH 2.5, A flow rate of 1.2 ml/min, UV detection at 265nm and attenuation of 0.02 aufs were performed. The system suitability was established, and the statistical validation of the performance was carried out for linearity, accuracy and precision. Different chromatograms were observed for the acid, base and photo-degraded samples. The results suggest that different degradation reaction followed different mechanism. The major different degradation products resulting from acid, base and photo-degradation of ketoprofen were separated by this HPLC method.

並列關鍵字

Ketoprofen ； HPLC ； validation