Optimization and validation of a high performance liquid chromatography method for rapid determination of sinafloxacin, a novel fluoroquinolone in rat plasma using a fused-core C(18)-silica column.
ABSTRACT A novel, simple and rapid high performance liquid chromatographic method has been developed and validated for the determination of sinafloxacin, a new fluoroquinolone, in rat plasma using 96-well protein precipitation, fused-core C(18)-silica column (4.6mmx50mm, 2.7microm) packed with a new solid support, which is made of 2.7microm particles that consist of a 1.7microm solid core covered with a 0.5microm thick shell of porous silica.The chromatographic separation was achieved with a mobile phase of 20:80 (v/v) of acetonitrile and phosphate buffer (pH=3.0) at a flow rate of 1mlmin(-1). Fluorescence detection was employed with lambda(ex) 295nm and lambda(em) 505nm. Lomefloxacin was used as internal standard (IS). The total analysis time was as short as 3min. The method was sensitive with a limit of detection (LOD) of 2ngml(-1), with good linearity (R(2)=0.9996) over the linear range of 5-500ngml(-1). The intra-day and inter-day precision was less than 5.8% and accuracy ranged from 100.3% to 103.5% for quality control (QC) samples at three concentrations of 10, 50 and 400ngml(-1).The fused-core C(18)-silica column method offered high sample throughput, low injection volume and low consumption of organic solvents. The method was successfully employed in the pharmacokinetic study of sinafloxacin formulation product after tail vein injection to healthy rats.
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ABSTRACT: As part of the method development, the injection volume as a critical quality attribute in fast fused-core chromatography was evaluated. Spilanthol, a pharmaceutically interesting N-alkylamide currently under investigation in our laboratory, was chosen as the model compound. Spilanthol was dissolved in both PBS and MeOH/H2O (70/30, v/v) and subsequently analyzed using a fused-core system hereby selecting five chromatographic characteristics (retention time, area, height, theoretical plates and symmetry factor) as responses. We demonstrated that the injection volume significantly influenced both the qualitative and quantitative performance of fused-core chromatography, a phenomenon which is confounded with the nature of the used sample solvent. From 2 μL up to 100 μL injection volume with PBS as solvent, the symmetry factor decreased favorably by 20%. Moreover, the theoretical plates and the quantitative parameters (area and height) increased up to 30%. On the contrary, in this injection volume range, the theoretical plates for the methanol-based samples decreased by more than 60%, while the symmetry factor increased and the height decreased, both by 30%. The injection volume is thus a critical and often overlooked parameter in fused-core method description and validation.Journal of Pharmaceutical Analysis. 01/2013; 3(5):330–334.
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ABSTRACT: A simple and rapid method for the determination of residues of four fluoroquinolones in blood samples was developed. The method was based on matrix solid-phase dispersion extraction followed by CE with ultraviolet detection. 1-Butyl-3-methylimidazolium tetrafluoroborate aqueous solution was used as the background electrolyte for the separation of fluoroquinolones. The average recoveries of the four fluoroquinolones at two spiked levels ranged from 54.0 to 86.4% for pig blood, and 45.4 to 79.9% for deer blood, with the relative standard deviations <9.45%. Detection limits for the four fluoroquinolones in blood sample ranged from 0.15 to 0.31 μg/mL.Journal of Separation Science 03/2011; 34(7):822-9. · 2.59 Impact Factor
- Journal of oral and maxillofacial surgery: official journal of the American Association of Oral and Maxillofacial Surgeons 08/2011; 70(5):1102-8. · 1.58 Impact Factor