title: Stability indicating methods for the determination of some fluoroquinolones in the presence of their decarboxylated degrades.
abstract: Two stability-indicating methods, namely densitometric TLC and derivative spectrophotometry for the determination of the fluoroquinolone antibacterials lomefloxacin (Lfx), moxifloxacin (Mfx), and sparfloxacin (Sfx) in the presence of their acid degrades are described. Acid degradation was adopted and the main decarboxylated product separated by TLC. Degradation products were identified confirming a previously mentioned degradation scheme. The densitometric method is based on the separation of the intact drug from its acid degradation product on silica gel G plates using different mobile phases and the spots of the intact drugs were scanned at 288, 290, and 292 nm for Lfx, Mfx, and Sfx, respectively. The derivative spectrophotometric method utilizes first derivative D(1) UV spectrophotometry with zero crossing points at 295.2 nm for Lfx, 280.4 and 303.4 nm for Mfx, and 280.8 nm for Sfx. Regression analysis of Beer's plots showed good correlation in the concentration ranges 0.2-1.2, 0.1-1.4, and 0.5-2.0 microg/spot for Lfx, Mfx, and Sfx, respectively, in the densitometric method and 2-16 microg/ml for all drugs in the derivative spectrophotometric method. The proposed methods were successfully applied for the determination of the investigated drugs in bulk powder with mean percentage accuracy ranges from 98.93 to 101.25% for the TLC method and from 98.18 to 100.35% for the D(1) method. The proposed methods were also applied for the determination of the investigated drugs in their pharmaceutical dosage forms and their validity was assessed using the standard addition technique with mean percentage recovery ranging from 100.25 to 101.70% in the TLC method and from 99.27 to 102.12% in the D(1) method. The selectivity of the proposed methods was tested by the analysis of laboratory-prepared mixtures containing different percentages of the studied drugs and their acid degrades. The proposed methods were found selective for the determination of the intact drugs in the presence of up to 90% of their degrades in the TLC method and 70% for Lfx and 90% for Mfx and Sfx in the D(1) method.
authors.affiliation: Analytical Chemistry Department, Faculty of Pharmacy, Cairo University, Cairo, Egypt. maissas@hotmail.com
authors.forename: Maissa Yacoub
authors.initials: MY
authors.lastname: Salem
authors.forename: Nabawia Mahmoud
authors.initials: NM
authors.lastname: El-Guindi
authors.forename: Hanaa Karam
authors.initials: HK
authors.lastname: Mikael
authors.forename: Laila El-Sayed
authors.initials: Lel-S
authors.lastname: Abd-El-Fattah
mesh_terms: D001372:Aza Compounds / Q000737:chemistry*; D002855:Chromatography, Thin Layer / Q000379:methods*; D003720:Densitometry / Q000379:methods*; D004355:Drug Stability; D024841:Fluoroquinolones / Q000737:chemistry*; D015394:Molecular Structure; D000077266:Moxifloxacin; D011804:Quinolines / Q000737:chemistry*; D013053:Spectrophotometry / Q000379:methods*
chemical_list: D001372:Aza Compounds; D024841:Fluoroquinolones; D011804:Quinolines; C053091:lomefloxacin; C061363:sparfloxacin; D000077266:Moxifloxacin