Vol.2, No.8, 828-840 (2010) Natural Science
doi:10.4236/ns.2010.28104
Copyright © 2010 SciRes. Openly accessible at http://www.scirp.org/journal/NS/
Spectophotometric method for determination of certain
cephalosporins using 4-chloro-7-nitrobenzo-2-oxa-1,
3-diazole (NBD-Cl)
Azza H. Rageh*, Salwa R. El-Shaboury, Gamal A. Saleh, and Fardous A. Mohamed
Department of Pharmaceutical Analytical Chemistry, Facutly of Pharmacy, Assiut University, Assiut, Egypt; *Corresponding Author:
azhesham@yahoo.com
Received 11 February 2010; revised 23 March 2010; accepted 30 March 2010.
ABSTRACT
A simple, accurate and precise spectropho-
tometric method has been proposed for the de-
termination of eleven cephalosporins, namely;
cefaclor monohydrate, cefadroxil monohydrate,
cefalexin anhydrous, cefradine anhydrous, ce-
fotaxime sodium, cefoperazone sodium, ceftri-
axone sodium, ceftazidime penthydrate, cefa-
zolin sodium, cefixime and cefpodoxime pro-
xetil in bulk drug and in pharmaceutical formu-
lations. The method depends on hydrolysis of
the studied drugs using 0.5M NaOH at 100°C
and subsequent reaction of the formed sulfide
ions with NBD-Cl (4-chloro-7-nitrobenzo-2-oxa-1,
3-diazole) to form a yellow-colored chromogen
measured at 390 nm. Different variables affect-
ing the reaction (e.g. NaOH concentration, hy-
drolysis time, NBD-Cl concentration and dilut-
ing solvent) were studied and optimized. Under
the optimum conditions, linear relationships
with good correlation coefficients (0.9990-
0.9999) were found in the range of 5-160 μg mL
-1
for all studied drugs. The limits of assay detec-
tion and quantitiation ranged from 0.289 to 5.867
and from 0.878 to 17.778 μg mL
-1
; respectively.
The accuracy and precision of the proposed
method were satisfactory. The method was suc-
cessfully applied for analysis of the studied
drugs in their pharmaceutical formulations and
the recovery percentages ranged from 96.6 to
103.5%.
Keywords: Spectrophotometry; Cephalosporins;
NBD-Cl; Pharmaceutical Analysis
1. INTRODUCTION
Cephalosporins have been used since 1948. These anti-
biotics have assumed a prominent role in modern antim-
icrobial therapy due to enhanced intrinsic microbiologi-
cal activities and favorable safety profile. Chemical
structures of cephalosporins drive from the 7-aminoce-
phalosporanic acid (7-ACA) composed of a β-lactam
ring fused with a dihydrothaizine ring (Figure 1), but
differ in the nature of substituents at the 3- and/or
7-positions of the cephem ring. These substituents affect
either the pharmacokinetic properties (3-position) or the
antibacterial spectrum (7-position) of the cephalosporins
[1,2]. Traditionally, cephalosporins are divided into first-,
second-, third-, and fourth-generation agents. Table 1
shows cephalosporins studied in this work. Several
methods have been reported for cephalosporins deter-
mination. The official procedures in pharmaceutical
preparations utilize high-performance liquid chromatog-
raphy (HPLC) [3] which is expensive. Other reported
procedures include spectrophotometric [4-9], spectro-
fluorimetric [10-13], chemiluminescence [14-16], chro-
matographic [17-20] and electrochemical methods [21-24]
and most of them are lengthy and/or tedious.
The hydrolytic degradation of cephalosporins was
very often used as a preliminary step in the analytical
procedure used for their determinations [25-32]. The
literature reveals that many spectrophotometric methods
were developed for cephalosporins determinations that
based on hydrolysis of these drugs using alkaline degra-
Figure 1. Chemical structure of 7-aminocephalosporanic acid.