Determination of gemifloxacin on dried blood spots by hydrophilic interaction liquid chromatography with fluorescence detector: application to pharmacokinetics in rats

Abstract

A highly selective, sensitive and rapid hydrophilic liquid interaction chromatographic method was developed and validated for determination of gemifloxacin on dried blood spots. The chromatographic separation was achieved on a reversed-phase zwitterionic hydrophilic interaction liquid chromatographic ZIC®HILIC-C₁₈ (4.6 × 100 mm; 5 µm) column using acetonitrile-10 mM ammonium acetate (pH 3.5; 80:20, v/v) as a mobile phase in an isocratic elution mode at a flow rate 0.6 mL/min at 27 °C. An on-line fluorescence detector set at excitation and emission wavelengths of 269 and 393 nm, respectively was used for monitoring column eluents. Ciprofloxacin was used as an internal standard. The method was validated for accuracy, precision, linearity and selectivity by design of experiments following ICH guidelines. The assay exhibited a linear range of 25-5000 ng/mL for gemifloxacin on dried blood spots. The lower limit of detection was found to be 10 ng/mL. The intra- and inter-assay coefficients of variation did not exceed 7.4% deviation of the nominal concentration. The recovery of GFX from dried blood spots was >95.0% and its stability was excellent with no evidence of degradation during sample processing for at least 3 months storage in a freezer at -20 °C.

Analytical Methods for Determining Third and Fourth Generation Fluoroquinolones: A Review

“…GEMI was analysed by HPLC and high performance thin layer chromatography (HPTLC). The HPLC methods involved FLD, UV, and PDA detection [ 72 , 92 – 94 ]. The HPTLC plates were detected in UV light [ 93 ].…”

“…The HPTLC plates were detected in UV light [ 93 ]. The applied columns were C18 [ 72 , 93 , 94 ] and HILIC [ 92 ]. As in the previously reported method the applied organic solvents were ACN [ 72 , 92 ], methanol [ 93 , 94 ].…”

“…The applied columns were C18 [ 72 , 93 , 94 ] and HILIC [ 92 ]. As in the previously reported method the applied organic solvents were ACN [ 72 , 92 ], methanol [ 93 , 94 ]. The aqueous solutions contained 10 mM ammonium acetate [ 92 ], 0.1% TFA [ 72 ], sodium acetate [ 93 ], orthophosphorc acid [ 93 ].…”

A very simple high‐performance liquid chromatographic method with fluorescence detection for the determination of gemifloxacin in human breast milk

“…Several reports in the literature have detailed the analysis of GEM by numerous methods using different biological matrices by high‐performance liquid chromatography (HPLC) and UV light , fluorescence or tandem mass spectrometry (MS/MS) detection. To our knowledge, however, there is currently no available method for determining GEM in breast milk samples.…”

Spectrofluorimetric analysis of gemifloxacin mesylate in pharmaceutical formulations

“…There have been few reported analytical methods for the estimation of GFX in pharmaceutical preparations or biological fluids namely, high‐performance liquid chromatography , high‐performance liquid chromatography–tandem mass spectrometry (LC–MS–MS) , capillary electrophoresis , voltammetry , chemiluminescence , spectrophotometry and spectrofluorimetry .…”