212
Summary
A simple and sensitive thin-layer chromatographic method has been
established for analysis of bupropion hydrochloride in pharmaceu-
tical tablets. Chromatography on silica gel 60 F
254
plates with
30:10:1 (v/v) ethanol–chloroform–glacial acetic acid as mobile phase
furnished compact spots at R
F
0.56 ± 0.01. Densitometric analysis
was performed at 254 nm. To show the specificity of the method
bupropion hydrochloride was subjected to acid and alkaline hydrol-
ysis, oxidation, photodegradation, and dry and wet heat treatment;
peaks of degradation products were well resolved from that of the
pure drug. Linear regression analysis revealed a good linear rela-
tionship between peak area and amount of bupropion hydrochlo-
ride in the range 200–1000 ng per band. The limits of detection and
quantitation were 11.45 and 34.71 ng per band, respectively. The
method was validated, in accordance with ICH guidelines, for preci-
sion, accuracy, robustness, and ruggedness. The intra-day and inter-
day repeatability of the method, as RSD, was approximately 1-2%,
showing method precision was sufficient. Method recovery was
between 102.07 and 104.58% and between 97.20 and 102.19% for
quality-control standards and for bupropion hydrochloride in a
synthetic mixture, respectively. Statistical comparison of results
with those obtained from HPLC analysis proved the method is
reproducible and enables selective analysis of bupropion hydrochlo-
ride in pharmaceuticals. Because the method could effectively sepa-
rate the drug from its degradation products, it can be regarded as
stability indicating.
1 Introduction
Bupropion hydrochloride (BUP), (±)-2-(tert-butylamino)-3’-
chloropropiophenone hydrochloride (Figure 1) is an aminoke-
tone derivative with a pK
a
of 7.9 [1]. It is a second-generation
antidepressant agent with neurochemical properties different
from those of conventional tricyclic antidepressants. It has been
reported that BUP is a selective inhibitor of neuronal reuptake of
catecholamines (noradrenalin and dopamine) with minimum
effect on reuptake of indolamines (serotonin) and no inhibitory
effect on monoamine oxidase. BUP in sustained release form is
used in smoking cessation as the first licensed non-nicotine
pharmacological therapy [2].
Several chromatographic methods have been reported for the
analysis of BUP in biological fluids, including high-perfor-
mance liquid chromatography (HPLC) [1, 3–6] and liquid chro-
matography–tandem mass spectrometry (LC–MS) [7]. Chiral
separation of the enantiomers of BUP on an ovomucoid column
has also been reported [8]. By use of Cooper’s method, the sta-
bility of BUP in human plasma and pharmacokinetic profiles in
different animal models have been determined [9, 10]. A few
chromatographic methods, including HPLC [11, 12], gas chro-
matography [13], and electrokinetic chromatography [14] have
been reported for analysis of BUP in pharmaceutical formula-
tions. A thin-layer chromatographic (TLC) method, in the BUP
monograph in USP XXIX, is available for analysis of its degra-
dation product, m-chlorobenzoic acid, and related impurities. In
this method, the spots were applied to 0.25-mm layer of high-
performance silica gel and chromatographed with the mobile
phase toluene–cyclohexane–glacial acetic acid 47:47:6 (v/v)
[15]. As we are aware, no TLC method for analysis of BUP in
pharmaceutical preparations has been reported in the literature.
The objective of this study was to establish, in accordance with
ICH guidelines [16], a simple, accurate, specific and repro-
ducible TLC method which could be used for analysis of BUP in
pharmaceutical preparations, in the presence of its degradation
products.
D. Yeniceli, D. Dogrukol-Ak, Anadolu University, Faculty of Pharmacy, Depart-
ment of Analytical Chemistry 26470 Eskisehir, Turkey.
E-mail: dak@anadolu.edu.tr
A Validated Thin-Layer Chromatographic Method for
Analysis of Bupropion Hydrochloride in a Pharmaceutical
Dosage Form
Duygu Yeniceli and Dilek Dogrukol-Ak*
Key Words
Bupropion hydrochloride
Thin-layer chromatography (TLC)
Method validation
Stability
Tablet analysis
Figure 1
Chemical structure of BUP.
Journal of Planar Chromatography 23 (2010) 3, 212–218 DOI: 10.1556/JPC.23.2010.3.9
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