Stability-Indicating LC Assay and Determination of System Suitability Limits with a Robustness Test of Gemifloxacin Mesylate in Tablets

Paim, Clésio Soldateli; Führ, Fernanda; Miron, Diogo; Pereira, Rúbia Lazzaretti; Malesuik, Marcelo Donadel; Steppe, Martin; Schapoval, Elfrides Eva Scherman

doi:10.2174/1573411011006040269

Cited by 8 publications

(18 citation statements)

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“…The purity of the degradation product was evaluated by LC (Fig. ) using the stability‐indication method previously validated (Paim et al ., ). The chromatographic peak purity tool, applied to the degradation product, demonstrated that the peak was pure, confirming the absence of other substances coeluting at the same retention time of 272 nm.…”

Section: Resultsmentioning

confidence: 99%

“…The literature researched describes the determination of GFM in biological fluids by liquid chromatography-mass spectrometry (LC-MS) (Allen et al, 2001;Doyle et al, 2000), liquid chromatography-electrospray tandem mass spectrometry (LC-ESI-MS-MS) (Robledo and Smyth, 2008), chiral separation (Hyun et al, 2002), chemiluminescence (Zhao et al, 2013) and in tablets by spectrophotometric method Sankar, 2008a, 2008b), LC (Paim et al, 2010;Rao et al, 2011), microbiological assay (Paim et al, 2011) and capillary electrophoresis (Paim et al, 2014).…”

Section: Introductionmentioning

confidence: 99%

“…Forced degradation studies on GFM were reported by Paim et al (2010Paim et al ( , 2011Paim et al ( , 2014 and degradation products were detected in photolytic (UV-A and UV-C radiation), acidic (0.1 mol L À1 HCl) and basic (0.01 mol L À1 NaOH) conditions. These studies are important to provide information to aid understanding of the degradation pathways of the drug and may indicate potential stability-critical impurities or potential phototoxicity issues with a given drug.…”

Section: Introductionmentioning

confidence: 99%

“…The ICH guidelines require stress testing of the drug substance to be performed, which can help to identify the likely degradation products and can be useful to establish degradation pathways and validate a stability-indicating method (ICH, 2003(ICH, , 2006a. The validated stability-indicating method previously developed by our research group was applied in the stability studies (Paim et al, 2010).…”

Section: Introductionmentioning

confidence: 99%

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Structural elucidation of gemifloxacin mesylate degradation product

Paim

Führ

Martins

et al. 2015

Biomedical Chromatography

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Gemifloxacin mesylate (GFM), chemically (R,S)-7-[(4Z)-3-(aminomethyl)-4-(methoxyimino)-1-pyrrolidinyl]-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylic acid methanesulfonate, is a synthetic broad-spectrum antibacterial agent. Although many papers have been published in the literature describing the stability of fluorquinolones, little is known about the degradation products of GFM. Forced degradation studies of GFM were performed using radiation (UV-A), acid (1 mol L(-1) HCl) and alkaline conditions (0.2 mol L(-1) NaOH). The main degradation product, formed under alkaline conditions, was isolated using semi-preparative LC and structurally elucidated by nuclear magnetic resonance (proton - (1) H; carbon - (13) C; correlate spectroscopy - COSY; heteronuclear single quantum coherence - HSQC; heteronuclear multiple-bond correlation - HMBC; spectroscopy - infrared, atomic emission and mass spectrometry techniques). The degradation product isolated was characterized as sodium 7-amino-1-pyrrolidinyl-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylate, which was formed by loss of the 3-(aminomethyl)-4-(methoxyimino)-1-pyrrolidinyl ring and formation of the sodium carboxylate. The structural characterization of the degradation product was very important to understand the degradation mechanism of the GFM under alkaline conditions. In addition, the results highlight the importance of appropriate protection against hydrolysis and UV radiation during the drug-development process, storage, handling and quality control.

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Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

Structural elucidation of gemifloxacin mesylate degradation product

Paim

Führ

Martins

et al. 2015

Biomedical Chromatography

View full text Add to dashboard Cite

show abstract

“…1). Few analytical methods appeared in the literature for the determination of this drug including spectrophotometric [21][22][23][24], LC [25][26][27], HPLC [28,29], electrophoresis [30,31] and spectrofluorimetry [32,33] were reported for analysis of GFX.…”

Section: Introductionmentioning

confidence: 99%