Validated HPLC determination of 2-[(dimethylamino)methyl]cyclohexanone, an impurity in tramadol, using a precolumn derivatisation reaction with 2,4-dinitrophenylhydrazine.
A new method for the determination of 2-[(dimethylamino)methyl]cyclohexanone (DAMC) in Tramadol (as active substance or active ingredient in pharmaceutical formulations) is described. The method is based on the derivatisation of 2-[(dimethylamino)methyl]cyclohexanone with 2,4-dinitrophenylhydrazine (2,4-DNPH) in acidic conditions followed by a reversed-phase liquid chromatographic separation with UV detection. The method is simple, selective, quantitative and allows the determination of 2-[(dimethylamino)methyl]cyclohexanone at the low ppm level. The proposed method was validated with respect to selectivity, precision, linearity, accuracy and robustness.
Medvedovici
Andrei
A
Department of Analytical Chemistry, Faculty of Chemistry, University of Bucharest, Sos. Panduri, no. 90-92, sect. 5, Bucharest, Romania. david@chem.unibuc.ro
Albu
Florin
F
Farca
Alexandru
A
David
Victor
V
D002851:Chromatography, High Pressure Liquid / Q000379:methods; D003512:Cyclohexanones / Q000032:analysis* / Q000737:chemistry; D004123:Dimethylamines / Q000032:analysis / Q000737:chemistry; D004340:Drug Contamination; D010659:Phenylhydrazines / Q000032:analysis* / Q000737:chemistry; D014147:Tramadol / Q000032:analysis* / Q000737:chemistry
D003512:Cyclohexanones; D004123:Dimethylamines; D010659:Phenylhydrazines; C004787:2,4-dinitrophenylhydrazine; D014147:Tramadol; C036468:cyclohexanone