Spectrofluorometry, thin layer chromatography, and column high-performance liquid chromatography determination of rabeprazole sodium in the presence of its acidic and oxidized degradation products.
The objective of this study is to develop validated stability-indicating spectrofluorometric, TLC-densitometric, and HPLC methods for the determination of rabeprazole sodium and its degradation products. The first method was based on measuring the fluorescence intensity of the drug at 416 and 311 nm for the emission and at 320 and 274 nm for the excitation for acid and oxidized solutions, respectively. The second method was based on the separation of the drug from its acidic and oxidized degradation products followed by densitometric measurement of the intact drug spot at 284 nm. The separation was carried out on Fluka TLC sheets of silica gel 60 F254 using isopropyl alcohol--30% ammonia (80 + 2, v/v) mobile phase. The third method was based on HPLC separation of rabeprazole sodium from its acidic and oxidized degradation products on a reversed-phase Waters Nova-Pak C18 column using 0.05 M potassium dihydrogen phosphate-methanol-acetonitrile (5 + 3 + 2, v/v/v) pH 7 +/- 0.2 mobile phase. The proposed procedures were successfully applied for the determination of rabeprazole sodium in pure form, laboratory-prepared mixtures, tablet, and expired batch. The obtained results were statistically compared with those of a reported method and validated according to United States Pharmacopeia guidelines. Two main acidic degradation products of the drug were separated and subjected to IR spectrometry and MS to confirm their structures, and the schemes for their formation were elucidated.
Osman
Afaf Osman
AO
National Organization for Drug Control and Research, 6 Abu Hazem St Pyramids, PO Box 29, Cairo, Egypt. afaf_osmanelteti@yahoo.com
Osman
Afaf
A
Osman
Mohamed
M
D053799:2-Pyridinylmethylsulfinylbenzimidazoles / Q000032:analysis* / Q000494:pharmacology*; D000097:Acetonitriles / Q000737:chemistry; D000438:Alcohols / Q000737:chemistry; D000641:Ammonia / Q000737:chemistry; D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D002855:Chromatography, Thin Layer / Q000379:methods*; D003720:Densitometry / Q000379:methods; D004791:Enzyme Inhibitors / Q000032:analysis / Q000494:pharmacology; D013058:Mass Spectrometry / Q000379:methods; D000432:Methanol / Q000737:chemistry; D010100:Oxygen / Q000737:chemistry; D004364:Pharmaceutical Preparations / Q000032:analysis; D010710:Phosphates / Q000737:chemistry; D017680:Potassium Compounds / Q000737:chemistry; D064750:Rabeprazole; D012822:Silicon Dioxide / Q000737:chemistry; D013050:Spectrometry, Fluorescence / Q000379:methods*; D013055:Spectrophotometry, Infrared / Q000379:methods
D053799:2-Pyridinylmethylsulfinylbenzimidazoles; D000097:Acetonitriles; D000438:Alcohols; D004791:Enzyme Inhibitors; D004364:Pharmaceutical Preparations; D010710:Phosphates; D017680:Potassium Compounds; D064750:Rabeprazole; D012822:Silicon Dioxide; D000641:Ammonia; C013216:potassium phosphate; D010100:Oxygen; D000432:Methanol; C032159:acetonitrile