Electrophoresis, Vol.32, No.16, 2155-2160, 2011
Capillary electrophoresis-electrochemiluminescence detection method for the analysis of ibandronate in drug formulations and human urine
A simple, rapid and sensitive CE method coupled with electrochemiluminescence (ECL) detection for direct analysis of ibandronate (IBAN) has been developed. Using a buffer solution of 20 mM sodium phosphate (pH 9.0) and a voltage of 13.5 kV, separation of IBAN in a 30-cm length capillary was achieved in 3 min. ECL detection was performed with an indium tin oxide working electrode bias at 1.6 V (versus a Pt wire reference) in a 200-mM sodium phosphate buffer (pH 8.0) containing 3.5 mM Ru(bpy)(3)(2+) (where bpy = 2,2'-bipyridyl).Derivatization of IBAN prior to CE-ECL analysis was not needed. Linear correlation (r = 0.9992, n = 7) between ECL intensity and analyte concentration was obtained in the range of 0.25-50 mM IBAN. The LOD of IBAN in water was 0.08 mu M. The developed method was applied to the analysis of IBAN in a drug formulation and human urine sample. SPE using magnetic Fe3O4@Al2O3 nanoparticles as the extraction phase was employed to pretreat the urine sample before CE-ECL analysis. The linear range was 0.2-12.0 mu M IBAN in human urine (r - 0.9974, n -6). The LOD of IBAN in urine was 0.06 mu M. Total analysis time including sample preparation was <1 h.