A Validated Stability-Indicating LC Method for Orbifloxacin in the Presence of Degradation Products

Cazedey, Edith Cristina Laignier; Othman, Asma; Garg, Sanjay; Salgado, Hérida Regina Nunes

doi:10.2174/157341211796353264

Cited by 7 publications

(4 citation statements)

References 22 publications

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“…ORBI quantification in the solubility test was performed by a stability-indicating method with high performance liquid chromatography as described by Casedey and collaborators [48]. The chromatographic separation was achieved using a Prominence model Shimadzu™ liquid chromatograph (Kyoto, Japan) with a DGU-20A 3R degasser, SIL-20AC HT autosampler, CTO-20A oven, LC-20AD pump, and SPD-M20A diode array detector.…”

Section: Methodsmentioning

confidence: 99%

Structure, Solubility and Stability of Orbifloxacin Crystal Forms: Hemihydrate versus Anhydrate

et al. 2016

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Orbifloxacin (ORBI) is a widely used antimicrobial drug of the fluoroquinolone class. In the official pharmaceutical compendia the existence of polymorphism in this active pharmaceutical ingredient (API) is reported. No crystal structure has been reported for this API and as described in the literature, its solubility is very controversial. Considering that different solid forms of the same API may have different physicochemical properties, these different solubilities may have resulted from analyses inadvertently carried out on different polymorphs. The solubility is the most critical property because it can affect the bioavailability and may compromise the quality of a drug product. The crystalline structure of ORBI determined by SCXRD is reported here for the first time. The structural analysis reveals that the ORBI molecule is zwitterionic and hemihydrated. ORBI hemihydrated form was characterized by the following techniques: TG/DTA, FTIR-ATR, and PXRD. A second crystalline ORBI form is also reported: the ORBI anhydrous form was obtained by heating the hemihydrate. These ORBI solid forms were isomorphous, since no significant change in unit cell and space group symmetry were observed. The solid-state phase transformation between these forms is discussed and the equilibrium solubility data were examined in order to check the impact of the differences observed in their crystalline structures.

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Section: Methodsmentioning

confidence: 99%

Structure, Solubility and Stability of Orbifloxacin Crystal Forms: Hemihydrate versus Anhydrate

et al. 2016

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“…Not informed [46] HPLC [47] (continued on next page) other fluoroquinolones, such as orbifloxacin, [53] norfloxacin, [54] and sparfloxacin. [55,56] Ultra-efficient liquid chromatography (U-HPLC), in turn, was used to analyze besifloxacin and other quinolones in cosmetics [57] and in a mixture of R-besifloxacin and S-besifloxacin enantiomers.…”

Section: Uv (289 Nm)mentioning

confidence: 99%

Besifloxacin: A Critical Review of Its Characteristics, Properties, and Analytical Methods

Tótoli

Salgado

2018

Critical Reviews in Analytical Chemistry

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Bacterial conjunctivitis has high impact on the health of the population, since it represents more than a third of ocular pathologies reported by health services worldwide. There is a high incidence of bacterial resistance to the antimicrobials most commonly used for the treatment of conjunctivitis. In this context, besifloxacin stands out, since it is a fluoroquinolone developed exclusively for topical ophthalmic use, presenting a low risk of developing resistance due to its reduced systemic exposure. Bausch & Lomb markets it as ophthalmic suspension, under the trade name Besivance™. Literature review on besifloxacin is presented, covering its pharmaceutical and clinical characteristics, and the analytical methods used to measure the drug in pharmaceutical products and biological samples. High performance liquid chromatography is the most used method for this purpose. A discussion on Green Chemistry is also presented, focusing the importance of the development of green analytical methods for the analysis of drugs.

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“…That a large number of methods using high performance liquid chromatography is available in the literature stems from the numerous advantages that the method provides (Salgado et al, 2005;Tozo, Salgado, 2006;Moreno, Salgado, 2008;Lopes, Salgado, 2009;Bonfilio et al, 2009;Cazedey et al, 2011;Corrêa et al, 2012;Silva, Salgado, 2012). Many methods described for CFZ up to the moment are directed to its quantification in biological matrices (Wold, 1977;Bayoumi et al, 1986;Nahata, 1990;Liang et al, 1994;Bompadre et al, 1998;Al-Rawithi et al, 2000;Samer, et al, 2000;Tsai, Chen, 2000;Arayne et al, 2007;Farthing et al, 2008), requiring pretreatment of the sample, among other slow procedures, requiring sophisticated equipment and high costs and using large amounts of organic solvents which are toxic for the operators and for the environment.…”

Section: Introductionmentioning

confidence: 99%

Validation of analytical methodology for quantification of cefazolin sodium pharmaceutical dosage form by high performance liquid chromatography to be applied for quality control in pharmaceutical industry

Pedroso

Salgado

2014

Braz. J. Pharm. Sci.

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A reversed-phase high performance liquid chromatography method was validated for the determination of cefazolin sodium in lyophilized powder for solution for injection to be applied for quality control in pharmaceutical industry. The liquid chromatography method was conducted on a Zorbax Eclipse Plus C 18 column (250 x 4.6 mm, 5 μm), maintained at room temperature. The mobile phase consisted of purified water: acetonitrile (60: 40 v/v), adjusted to pH 8 with triethylamine. The flow rate was of 0.5 mL min -1 and effluents were monitored at 270 nm. The retention time for cefazolin sodium was 3.6 min. The method proved to be linear (r 2 =0.9999) over the concentration range of 30-80 µg mL -1 . The selectivity of the method was proven through degradation studies. The method demonstrated satisfactory results for precision, accuracy, limits of detection and quantitation. The robustness of this method was evaluated using the Plackett-Burman fractional factorial experimental design with a matrix of 15 experiments and the statistical treatment proposed by Youden and Steiner. Finally, the proposed method could be also an advantageous option for the analysis of cefazolin sodium, contributing to improve the quality control and to assure the therapeutic efficacy.Uniterms: Cefazolin sodium/determination. High performance liquid chromatography/reverse-phase/ quantitative analysis. Pharmaceutical industry/quality control. Cefalosporine/quality control. Medicines/ quality control.Um método cromatográfico em fase reversa foi validado para a determinação de cefazolina sódica em pó liofilizado, a ser aplicado no controle de qualidade em indústrias farmacêuticas. O método por cromatografia líquida foi conduzido em coluna Zorbax Eclipse Plus C18 (250 × 4,6 mm, 5 µm) mantida à temperatura ambiente. A fase móvel consistiu de água purificada: acetonitrila (60 : 40 v/v), com o pH ajustado para 8 com trietilamina. A vazão usada foi de 0,5 mL min -1 e os analitos de interesse foram monitorizados a 270 nm. O tempo de retenção da cefazolina sódica foi de 3,6 min. As áreas dos picos de cefazolina sódica foram lineares na faixa de concentração de 30-80 µg mL -1 (r 2 = 0,9999). A seletividade do método foi demonstrada através de estudos de degradação. O método demonstrou resultados satisfatórios para precisão, exatidão, limites de detecção e de quantificação. A robustez do método foi avaliada utilizando o esquema fatorial de Plackett-Burman com uma matriz de 15 experimentos simultâneos, e analisados por tratamento estatístico proposto por Youden e Steiner. Finalmente, o método proposto pode ser também uma opção de êxito para a análise de cefazolina sódica, contribuindo para o controle de qualidade e para garantir a eficácia terapêutica.Unitermos: Cefazolina sódica/determinação. Cromatografia líquida de alta eficiência/fase reversa/ análise quantitativa. Indústria farmacêutica/controle de qualidade. Cefalosporina/controle de qualidade. Medicamentos/controle de qualidade.

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A Validated Stability-Indicating LC Method for Orbifloxacin in the Presence of Degradation Products

Cited by 7 publications

References 22 publications

Structure, Solubility and Stability of Orbifloxacin Crystal Forms: Hemihydrate versus Anhydrate

Structure, Solubility and Stability of Orbifloxacin Crystal Forms: Hemihydrate versus Anhydrate

Besifloxacin: A Critical Review of Its Characteristics, Properties, and Analytical Methods

Validation of analytical methodology for quantification of cefazolin sodium pharmaceutical dosage form by high performance liquid chromatography to be applied for quality control in pharmaceutical industry

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