Institution: | aBiocatalysis Laboratory, Department of Pharmaceutical Technology, National Institute of Pharmaceutical Education and Research, Sector 67, S.A.S. Nagar 160062, India bDepartment of Pharmaceutical Analysis, National Institute of Pharmaceutical Education and Research, Sector 67, S.A.S. Nagar 160062, India |
Abstract: | A simple reversed-phase high-performance liquid chromatographic method employing C-18 column has been developed for simultaneous analysis of three intermediates in the synthesis of S-duloxetine, the antidepressant drug, viz., 2-acetyl thiophene (AT), N,N-dimethyl-3-keto-(2-thienyl)-propanamine (DKTP) and (S)-N,N-dimethyl-3-hydroxy-(2-thienyl)-propanamine (DHTP). Good separations were achieved by employing an isocratic system using acetonitrile and 0.05 M phosphate buffer (pH 7.0) containing 0.02% diethylamine. The detection was carried out at 241 nm. The method was validated for linearity, range, accuracy and precision. The developed method was applied for monitoring the progress of chemical synthesis of DKTP from AT followed by the biocatalytic reduction of DKTP to DHTP as the disappearance of the substrate and formation of the product can be monitored simultaneously by the present method. |