SIMULTANEOUS SEPARATION AND DETERMINATION OF QUINOLONES IN PHARMACEUTICALS BY MICELLAR LIQUID CHROMATOGRAPHY

Abstract

A rapid and simple liquid chromatographic procedure using micellar mobile phases is reported for the separation and determination of four quinolones (pipemidic acid, levofloxacin, norfloxacin, and moxifloxacin) in pharmaceuticals.

This purpose was achieved without any previous pretreatment step in a C₁₈ column using a micellar mobile phase of 0.15 M sodium dodecyl sulphate, 2.5% propanol, and 0.5% triethylamine at pH 3, with retention times below 12 min. For detection, the diode-array UV-Vis set at 276 nm was used. The limits of detection and quantification were between 8 − 51 and 28 − 171 ng/mL, respectively. This method was validated in terms of intra-day and inter-day precision and accuracy, and robustness. Calibration curves over the concentration range of 0.1 − 50 μg/mL were linear (r² > 0.9997). Good claim percentages (96 − 106%) were obtained in the analysis of pharmaceutical formulations. The results show that the procedure is suitable for the routine analysis of drugs.

Keywords:

• direct injection
• micellar mobile phase
• pharmaceutical formulation
• quinolone
• SDS

ACKNOWLEDGMENTS

This work was supported by projects P1-1B2006-12 and CTQ2007-64473/BQU, funded by Foundation Caixa Castelló-Bancaixa-Universitat Jaume I and the Ministerio de Educación y Ciencia (MEC), respectively. Maria Rambla-Alegre also wishes to thank the MEC for the FPU grant.

Notes

^a n = 6.

^b n = 5.