50
INTERNATIONAL JOURNAL of BIOMEDICAL SCIENCE
Spectrophotometric Determination of Diazepam
in Pure Form, Tablets and Ampoules
W. F. El-Hawary, Y. M. Issa, A. Talat
Chemistry Department, Faculty of Science, Cairo University, Giza, Egypt
ABSTRACT
The interaction of diazepam with picric acid (I), 3,5-dinitrobenzoic acid (II) and 2,4-dinitrobenzoic acid
(III) was found to be useful for its spectrophotometric determination. The quantitation was carried out at
475, 500, and 500 nm for the reaction with (I), (II) and (III), respectively. The effect of several variables on
the coloring process was studied. The proposed methods have been applied successfully for the determina-
tion of diazepam in pure samples and in its pharmaceutical preparations with good accuracy and precision.
The results were compared to those obtained by the pharmacopoeial methods. The linear ranges for obedi-
ence of Beer’s law are up to 85.6, 180.2, and 128.6 μg/ml, Ringbom ranges are 10.0-79.0, 15.2-177.8, 17.0-83.0
μg/ml, and RSD 0.048, 0.028, and 0.026% for reaction of diazepam with I, II, and III, respectively.
Keywords: diazepam; 2,4-dinitrobenzoic acid; 3,5-dinitrobenzoic acid; picric acid; spectrophotometric
determination
Corresponding author: Y. H. Issa, Chemistry Department, Fac-
ulty of Science, Cairo University, Giza, Egypt. Tel: 00202-5676579; Fax:
+5728843; E-mail: yousrymi@yahoo.com.
Copyright: © 2007 W. F. El-Hawary et al. This is an open-access article
distributed under the terms of the Creative Commons Attribution Li-
cense (http://creativecommons.org/licenses/by/2.5/), which permits unre-
stricted use, distribution, and reproduction in any medium, provided the
original author and source are credited.
IntRoDuctIon
Diazepam (C
16
H
13
ClN
2
O) [7-chloro-1,3-dihydro-
1-methyl-5-phenyl-2H-1,4-benzodiazpein], M. Wt. 284.75
[CAS (439-14-5)] is an important compound widely used
therapeutically because of its relaxant, sedative, hypnotic
and anticonvulsant properties.
Several analytical procedures have been adapted for
the assay of diazepam. They include non-aqueous titra-
timetry (1, 2), ultraviolet spectrophotometry (3-5), vis-
ible spectrophotometry (6-10), second order-derivative
spectrophotometry (11, 12), fluorimetry (13, 14), high
performance liquid chromatography HPLC (15-17), gas
chromatography (18, 19), thin layer chromatography
(20), polarography (21, 22), potentiometry (23, 24) and
infrared assay (25). The official methods involve a non-
aqueous titration of diazepam by perchloric acid in acetic
anhydride medium using Nile blue as indicator (2) and
HPLC (17).
Most of the old colorimetric methods involve hydroly-
sis of the benzodiazepine moiety to benzophenones, and
thus lack specificity since this is the usual degradation
pathway of benzodiazepines, and other needs solvent ex-
traction before measurements. Therefore, a simple spec-
tro-photometric method for determination of diazepam is
needed. This is fulfilled in the present investigation by the
application of Zimmermann reaction to the active methy-
lene group adjacent to a carbonyl group in diazepam to
produce highly absorbing s-complexes (26) upon reaction
with picric acid (I), 3,5-dinitrobenzoic acid (II) and 2,4-di-
nitrobenzoic acid (III), respectively. The present study de-
scribes the spectrophotometric determination of diazepam
in pure samples and in its pharmaceutical preparations.
EXPERIMENTAL
Apparatus
Perkin Elmer Spectrophotometer model Lambda 1,
Hanna instrument coductometer model HI8819N and
ORIGINAL ARTICLE