Imipramine hydrochloride (IPM) is a tricyclic antidepressant [1] . Its chemical name is 10,l1-dihydro-5Hdibenz[b,f]azepine-5-(dimethylaminopropy1) hydrochloride. The molecular formula is C 19 H 24 N 2 . HCl and the molecular mass is 316.9 g/mol. It is officially recognized in Indian Pharmacopoeia (IP) [1] , British Pharmacopoeia (BP) [2] and the United States Pharmacopoeia (USP) [3] . Diazepam (DZM) an antianxiety, antiepileptic drug with the IUPAC name, 7-chloro-1,3-dihydro-1-methyl-5-phenyl-2H-1,4-benzodiazepin-2-one. The molecular formula of diazepam is C 16 H 13 ClN 2 O and the molecular weight is 284.7 g/mol. It is also officially recognized in IP [1] , BP [2] and USP [3] .IPM was studied as a single drug and in combination with other drugs [4][5][6] . Different methods like secondorder derivative spectrophotometry [5] , chemometric method [6] , spectrophotometry [7,8] , high performance liquid chromatography (HPLC) [4,9,10] , fluorescence polarization immunoassay [10] , HPLC-diode array detection (HPLC-DAD) [11] , surface ionization organic mass spectrometry [12] and HPLC tandem mass spectrometry (HPLC-MS/MS) [13] have been employed to measure IPM. It was also determined in human serum [4,9,13] and urine [4,9] . Diazepam has been studied separately, in combination with other benzodiazepines and other drugs [14][15][16][17][18][19][20] and its metabolites [21] . It was studied in whole blood [16] , plasma [17,18] , urine, hair and oral fluids [19,22] and in pharmaceutical form [23][24][25][26] . These studies were carried out using analytical methods such as secondderivative spectrophotometry [5] , chromatography [15] , HPLC [16][17][18]26] , LC-MS/MS [18,19] , HPLC electrospray tandem mass spectrometry [20] , capillary electrophoresis