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2 Acta Chromatographica

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Validated stability-indicating RP-HPLC UV method for simultaneous determination of metformin and repaglinide

Joshi S. S, Nahire R. R, Shastri N. R, Surendranath K. V, Satish J

Acta Chromatographica

2012

Vol. 24, no. 3

419--432

A simple, rapid, precise, and accurate, stability-indicating reversed phase high performance liquid chromatographic method was developed and validated for simultaneous determination of metformin HCl and repaglinide. The chromatographic separation was achieved on YMC Pack AM ODS (5 μm, 250 mm length × 4.6 mm i.d.) column at a detector wavelength of 210 nm, using an isocratic mobile phase consisting of methanol and 10 mM potassium dihydrogen phosphate buffer (pH 2.5) in a ratio of 70:30 v/v at a flow rate of 1 mL min-1. The retention times for metformin and repaglinide were found to be 2.6 and 11.3 min, respectively. The drugs were exposed to thermal, photolytic, hydrolytic, and oxidative stress conditions, and the stressed samples were analyzed by the proposed method. Validation of the method was carried out as per International Conference on Harmonization (ICH) guidelines. Linearity was established for metformin and repaglinide in the range of 5–200 μg mL-1 and 1–200 μg m-1. L, respectively. The limits of detection were 0.3 μg mL-1 and 0.13 μg mL-1 for metformin and repaglinide, respectively. The method was found to be specific and stability-indicating as no interfering peaks of degradants and excipients were observed. The proposed method is hence suitable for application in quality-control laboratories for quantitative analysis of both the drugs individually and in combination, since it is simple and rapid with good accuracy and precision.

Development and validation of a stability-indicating UHPLC method for assay of felbamate and related substances

Shetty S. K, Surendranath K. V, Kaja R. K., Satish J, Jogul J, Manitripathi U

Acta Chromatographica

2010

Vol. 22, no. 2

161--172

A new, sensitive, stability-indicating, and cost and time-effective isocratic reversed-phase UHPLC method has been developed for quantitative analysis of felbamate, an antiepileptic drug, both in the bulk drug and in pharmaceutical dosage forms. Chromatographic separation of felbamate and its two impurities was achieved on a C 18 column with a simple buffer-methanol mobile phase; the run time was 8 min. Quantification was achieved by ultraviolet detection. Resolution between the impurities was >2.0. Response was a linear function of concentration over the range 0.1–3.0 μg mL -1, correlation coefficient >0.999, for felbamate and the impurities. The method is capable of detecting the two impurities at levels of 0.002% (0.02 μg mL -1) of the test concentration of 1.0 mg mL -1 (1 μL injection). The same sensitivity was achieved for all the degradation products formed during stress studies in which the drug was subjected to hydrolysis, oxidation, photolysis, and thermal degradation. Substantial degradation occurred under acidic and basic conditions. The stressed test solutions were assayed against felbamate working standard and the mass balance in each case was close to 100%, indicating the method is stability-indicating. The method was validated for linearity, accuracy, precision, and robustness in accordance with ICH Guidelines.