Abstract

ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF RESIDUAL SOLVENTS IN METHOCARBAMOL BY GAS CHROMATOGRAPHY (GC/FID) WITH HEAD SPACE

Jyothsna Modugula* and Podili Venkata seshagiri

ABSTRACT

An analytical method for the quantification of residual solvents in Methocarbamol was established using a static headspace gas chromatography (HSGC) coupled with a flame ionization detector (FID). Methanol, IPA, Toulene and Benzene as residual solvents determined in Methocarbamol. Analysis was performed by headspace GC/FID method on Agilent 7890A system. Nitrogen was used as carrier gas with constant flow rate of 4.5 mL/min and the separation of residual solvents were achieved on DB-624 column. The thermostat temperature was 50°C-hold for 8 min-raise @ 10°C/min to 2300C for 10 min. The %RSD for six injections obtained are with in acceptance criteria. The percentage recovery ranges obtained from 94% and 108%.The correlation coefficients obtained are greater than 0.99. The method parameters were validated included specificity, limit of detection and quantification, accuracy, linearity, precision, and robustness. A new, simple, specific, accurate and precise method was validated according to the International Conference on Harmonization (ICH) guidelines.

Keywords: Methocarbamol, Validation, GC/FID, Residual Solvents, ICH.