Stability indicating reversed-phase liquid chromatographic determination of metronidazole benzoate and diloxanide furoate as bulk drug and in suspension dosage form.
A selective, precise and accurate isocratic RP-HPLC method has been developed and validated for the simultaneous determination of metronidazole benzoate (MB), diloxanide furoate (DF), methyl paraben (MPn) and propyl paraben (PPn) in suspension. The cis/trans isomerization phenomenon for DF has also been presented. The method uses as stationary phase a Supelco LC-18 DB (15 cm x 4.6 mm) 5 microm column and as a mobile phase a buffer-acetonitrile mixture (70:30, v/v) adjusted to pH of 2.5 at a flow rate of 2.0 mLmin(-1). The buffer is a 0.005 M KH2PO4 solution. The four analytes were well resolved from the degraded solutions peaks. The excepients present in the formulation do not interfere with the assay procedure. The linearity range (n=3) is (0.20130-1.20779 mgmL(-1)) for MB with R of 0.99985; (0.15790-0.94740 mgmL(-1)) for DF with R of 0.99987; (0.01131-0.06788 mgmL(-1)) for MPn with R of 0.99987 and (0.00126-0.00756 mgmL(-1)) for PPn with R of 0.99991. Precision (n=6) was 0.87% for MB; 1.15% for DF; 1.32% for MPn and 1.27% for PPn. The percentage recoveries (n=3) were 99.1% for MB; 99.6% for DF; 99.1% for MPn and 98.7% for PPn. The proposed method can be utilized for the routine analysis of the four analytes in pharmaceutical dosage form.
Mishal
Adel
A
Hikma Pharmaceuticals, Analytical Research, P.O. Box 182400, Amman 11118, Jordan. mishal@hikma.com
Sober
Diana
D
D001565:Benzoates / Q000737:chemistry; D002021:Buffers; D002138:Calibration; D002626:Chemistry, Pharmaceutical / Q000379:methods*; D002845:Chromatography; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004304:Dosage Forms; D004355:Drug Stability; D005663:Furans / Q000032:analysis* / Q000737:chemistry; D006863:Hydrogen-Ion Concentration; D008795:Metronidazole / Q000032:analysis* / Q000737:chemistry; D008956:Models, Chemical; D010226:Parabens / Q000032:analysis; D004364:Pharmaceutical Preparations / Q000032:analysis*; D010919:Placebos; D015203:Reproducibility of Results; D012997:Solvents; D013237:Stereoisomerism; D013997:Time Factors
D001565:Benzoates; D002021:Buffers; D004304:Dosage Forms; D005663:Furans; D010226:Parabens; D004364:Pharmaceutical Preparations; D010919:Placebos; D012997:Solvents; D008795:Metronidazole; C015358:methylparaben; C004932:diloxanide furoate; C006068:propylparaben