Validation of a capillary zone electrophoresis method for the determination of ciprofloxacin, gatifloxacin, moxifloxacin and ofloxacin in pharmaceutical formulations

Abstract

Um método alternativo por eletroforese capilar de zona (CZE) para determinação de ciprofloxacina (CPFLX), gatifloxacina (GTFLX), moxifloxacina (MFLX) e ofloxacina (OFLX) foi validado. O sistema de eletrólito utilizado consistiu da mistura de 25 mmol L -1 de TRIS/ HCl e 15 mmol L -1 de tetraborato de sódio em meio aquoso resultando em pH 8,87. A análise foi realizada sob detecção direta por UV em 282 nm com tempo de análise de 3 min. Os parâmetros analíticos de validação avaliados foram: linearidade (r > 0,998), seletividade (comparação entre a inclinação da curva de calibração de padronização externa e curva de calibração de adição de padrão), repetitividade em área para amostras (RSD %: < 3,94% para CPFLX, < 3,87% para GTFLX, 1,30% para MFLX e < 1,88% para OFLX), precisão intermediária em área para amostras (RSD%: < 3,59% para CPFLX, < 3,09% para GTFLX, 2,67% para MFLX e < 2,25% para OFLX), exatidão (média da faixa de recuperação: 101,2% para CPFLX, 101,0% para GTFLX, 101,3% para MFLX e 99,9% para OFLX), limite de detecção (mg L -1 : 2,72 para CPFLX, 1,92 para GTFLX, 0,795 para MFLX e 1,05 para OFLX), limite de quantificação (mg L -1 : 9,06 para CPFLX, 6,40 para GTFLX, 2,65 para MFLX e 3,50 para OFLX) e robustez. Devido à simplicidade, seletividade, precisão, exatidão e rapidez, o método pode ser uma alternativa interessante para auxiliar o controle da qualidade dessas drogas na indústria farmacêutica.An alternative capillary zone electrophoresis (CZE) method for the determination of ciprofloxacin (CPFLX), gatifloxacin (GTFLX), moxifloxacin (MFLX) and ofloxacin (OFLX) through a simple aqueous electrolyte system consisting of 25 mmol L -1 of TRIS/ hydrochloride and 15 mmol L -1 of sodium tetraborate buffer mixture (pH 8.87) using direct UV detection at 282 nm within 3 min was validated. The analytical parameters of validation evaluated were: linearity (r > 0.998), selectivity (comparison between slope of the calibration curve of external standard and calibration curve of standard addition), repeatability in area for sample (RSD%: < 3.94% for CPFLX, < 3.87% for GTFLX, 1.30% for MFLX and < 1.88% for OFLX), intermediate precision in area for sample (RSD%: < 3.59% for CPFLX, < 3.09% for GTFLX, 2.67% for MFLX and < 2.25% for OFLX), accuracy (mean of recovery range: 101.2% for CPFLX, 101.0% for GTFLX, 101.3% for MFLX and 99.9% for OFLX), limit of detection (mg L -1 : 2.72 for CPFLX, 1.92 for GTFLX, 0.795 for MFLX and 1.05 for OFLX), limit of quantification (mg L -1 : 9.06 for CPFLX, 6.40 for GTFLX, 2.65 for MFLX and 3.50 for OFLX) and robustness. Due to its simplicity, selectivity, precision, accuracy and rapidity, the methodology can be an interesting alternative for quality assurance in the pharmaceutical industry of these drugs.

Simultaneous separation of ciprofloxacin, norfloxacin and ofloxacin by micellar electrokinetic chromatography

“…10 The pKa values of the three compounds are presented in Table 1. 4,5,8 Initial runs were carried out to assess the feasibility of borate and phosphate buffers as background electrolytes. These preliminary experiments showed better results when using a buffer containing sodium tetraborate (pH 9.3) in order to obtain high resolution within shortest analysis time.…”

“…3 CE proved to be an important tool in the analysis of FQ derivatives but the large majority of the developed methods describe separation of FQs from different generations having different physicochemical characteristics. [4][5][6][7][8] Ciprofloxacin (CIP), norfloxacin (NOR) and ofloxacin (OFL) (three 2 nd generation FQs) are by far the important and widely used FQs. CIP and NOR have almost similar structural characteristics, the substituent at the nitrogen atom from the pyridin-carboxilic ring (cyclopropyl and ethyl side chain, respectively) being the only difference between the two, while OFL is a tricyclic derivative and has a methyl substituent on the piperazine ring ( Figure 1).…”

Adsorptive Stripping Voltammetric Determination of Oxolinic Acid in Water Sample

“…8 This antimicrobials agents are fairly tolerable to humans and can be widely used against mycobaterial and anaerobic organisms, acting by the inhibition of bacterial enzymes DNA gyrase and topoisomerase IV. 9 The first antibiotic agent of the quinolone class was synthesized in the laboratory in the 1960s by obtaining nalidixic acid as a by-product synthesis of antimalarial compounds synthesis. 10 Since then, structural modifications have resulted in the second, third and fourth generations of quinolones and fluoroquinolones, which are effective against Gram-negative and Gram-positive bacteria, being more powerful and featuring a wide activity spectrum.…”

Sensitive Spectrofluorimetric Method for Determination of Fluoroquinolones through Charge-Transfer Complex Formation

“…Thorough study of the literature reveals that several methods have been developed for the determination of fluoroquinolones in bulk, pharmaceutical dosage form and biological samples based on wide array of instru-ments like spectrophotometric [9][10][11], HPLC [12,13], capillary electrophoresis [14], electrochemical [15] and spectrofluorimetric [8,[16][17][18][19][20].…”