Chromatographic methods development, validation and degradation characterization of the antithyroid drug Carbimazole.

The current paper reports the development and validation of stability-indicating HPLC and HPTLC methods for the separation and quantification of main impurity and degradation product of Carbimazole. The structures of the degradation products formed under stress degradation conditions, including hydrolytic and oxidative, photolytic and thermal conditions, were characterized and confirmed by MS and IR analyses. Based on the characterization data, the obtained degradation product from hydrolytic conditions was found to be methimazole-impurity A of Carbimazole as reported by the British Pharmacopeia and the European Pharmacopeia. A stability-indicating HPLC method was carried out using a Zorbax Eclipse Plus CN column (150 × 4.6 mm i.d, 5 µm particle size) and a mobile phase composed of acetonitrile-0.05 m KH2 PO4 (20: 80, v/v) in isocratic elution, at a flow rate of 1 mL/min. The method was proved to be sensitive for the determination down to 0.5% of Carbimazole impurity A. Additionally, a stability-indicating chromatographic HPTLC method was achieved using cyclohexane-ethanol (9:1, v/v) as a developing system on HPTLC plates F254 with UV detection at 225 nm. The proposed HPLC and HPTLC methods were successfully applied to Carbimazole® tablets with mean percentage recoveries of 100.12 and 99.73%, respectively.

Kinetic determination of carbimazole, methimazole and propylthiouracil in pharmaceuticals, animal feed and animal livers.

Kinetic methods are proposed for the determination of carbimazole(CBZ), methimazole(MMI) and propylthiouracil(PTU) based on their inhibitory effects on the palladium(II)-catalysed reaction between the pyronine G and hypophosphite ions. The reactions are monitored spectrophotometrically at 548 nm. The influence of reaction variables and the interfering effect of other substances were studied. Under the selected experimental conditions (CBZ: 3.6 x 10(-5) mol l-1 pyronine G; pH 3.0; 0.7 microgram ml-1 PdII and 0.2 mol l-1 H2PO2-; MMI: 6 x 10(-5) mol l-1 pyronine G, pH 3.0; 0.7 microgram ml-1 PdII, 0.4 mol l-1 H2PO2-; PTU: 3.6 x 10(-5) mol l-1 pyronine G; pH 3.0; 0.7 microgram ml-1 PdII and 0.3 mol l-1 H2PO2-), these three antithyroids were determined in the following ranges: CBZ, 0.04-0.70 microgram ml-1; MMI, 0.04-0.50 microgram ml-1; PTU 0.08-1.00 microgram ml-1. The methods were applied to the determination of CBZ, MMI and PTU, in pharmaceuticals, animal feed and animal livers.