Development and Validation of HPLC and HPTLC Methods for Determination of Cefoperazone and Its Related Impurities.

Abstract

Validated sensitive and highly selective methods were developed for the quantitative determination of cefoperazone sodium (CEF) in the presence of its reported impurities; 7-aminocephalosporanic acid (7-ACA) and 5-mercapto-1-methyl-tetrazole (5-MER). Method A is high-performance liquid chromatography (HPLC), where the mixture of CEF and the reported impurities; 7-ACA and 5-MER were separated on a C8 column (5 µm ps, 250 mm × 4.6 i.d.) using methanol:0.05 M KH2PO4 buffer (22.5:77.5 v/v, pH 7.5) as a mobile phase. The three components were detected at 254 nm with a concentration range of 10-90 µg mL(-1) and the mean percentage recovery 99.67% (SD 1.465). Method B is high-performance thin layer chromatography (HPTLC), where the mixture of CEF and the reported impurities were separated on silica gel HPTLC F254 plates using (acetone:methanol:ethyl acetate:2% sodium lauryl sulfate:glacial acetic acid) (3:2:3:0.8:0.2, by volume) as a developing system and scanning at 254 nm over a concentration range of 1-10 µg per band with the mean percentage recovery 99.95% (SD 1.335). The proposed methods were statistically compared with a reported HPLC method with no significant difference regarding accuracy and precision; indicating the ability of the proposed methods to be reliable and suitable for routine analysis of drug product. The proposed HPTLC method proved to be more sensitive, while the HPLC gave more reproducible results besides saving time.