Abstrakt

Preparation and evaluation of molecularly imprinted polymer liquid chromatography column for the determination of enantiomeric impurity of l-Ephedrine sulfate-validated methods according to the ICH guidelines

Krishnamoorthy Balamurugan, Kannan Gokulakrishnan

Asensitive, simple, specific, precise, accurate and ruggedmethod for determination of enantiomeric impurity of l-Ephedrine Sulfate (l-EPS) a drugs substance has been developed. The separation of enantiomer is by molecularly imprinted polymer (MIP) column. In this study molecular imprinting technology was employed to prepare a specific affinity sorbent for the resolution of Ephedrine Sulfate (commonly used as a decongestant). The separation of isomer is by molecularly imprinted polymer (MIP) column 250mmï‚´ 4.6mmwith 10µ particle size. Column was maintained at 10ï‚°C.The UV/Vis detector was operated at 254nm. Flowrate of the mobile phase was 0.8ml/min. The method offers excellent separation of two enentiomers with resolution (R) is not less than 2 and tailing factor not more than 3.5. The method was validated for the quantification of d-Ephedrine enantiomer impurity (d-EPS) in the bulk drug l-Ephedrine Sulfate (l-EPS), was performed according to the International Conference on Harmonization (ICH) guidelines[ 1-4]. Calibration curves showed excellent linearity over the concentration range 0.025mg/ml to 0.1mg/ml (50% to 200 %) for d-EPS 0.05mg/ml (0.5%with respect to test concentration 10mg/ml). Precision of the method the relative standard deviationwas 0.99%limit of detection (LOD) and limit of quantification (LOQ) of the method for d-EPS were 0.2% and 0.5% respectively. Average recovery of the d-EPS was between 87.3% to 107.8%. This method was employed in determining enantiomeric impurity of bulk drug l-EPS.