Original Article
RAPID ASSAY DEVELOPMENT OF DICLOFENAC SODIUM COATED TABLET ASSAY USING FTIR
COMPARED TO HPLC METHOD
ILMA NUGRAHANI
1
, NOVENSIUS DILLEN
1
1
School of Pharmacy, Bandung Institute of Technology, Indonesia
Email: ilma_nugrahani@fa.itb.ac.id
Received: 06 Mar 2018, Revised and Accepted: 13 Apr 2018
ABSTRACT
Objective: A lot of coated tablet preparations of diclofenac have been marketed. This research aimed to develop and validate a quantitative analysis
method for diclofenac sodium coated tablet using Fourier Transform Infrared (FTIR), which never reported.
Methods: The quantification was done by measuring the sample spectra, which then was converted into its derivative. Areas under the curve (AUC)
of the derivative spectrums were plotted against the concentrations; corresponding to the calibration graphic. Then, the validation method was
carried out by evaluating the accuracy, precision, linearity, range, limit of detection (LOD), and limit of quantification (LOQ).
Results: The results showed that diclofenac sodium had a specific peak within the wavenumber range of 1550-1605 cm
-1
. This area showed
linearity to concentration within the range 0.1-1.0% w/w, with coefficient correlation of 0.9998. Recovery was found within 98-102% w/w. The
intra and inter-day precision showed a coefficient of variance below 2%. The LOD and LOQ were 0.0127% and 0.0424% respectively. Further, a
comparative study was performed, between this method and the compendia method using HPLC. The results showed that the measurement method
using FTIR has an advantage in terms of time and cost.
Conclusion: Based on all data, it is concluded that FTIR can be used as a valid alternative method. It is faster and more cost-effective for diclofenac
sodium coated tablet content determination, compared to the compendia method.
Keywords: Assay, Comparative study, Diclofenac sodium, FTIR, HPLC
© 2018 The Authors. Published by Innovare Academic Sciences Pvt Ltd. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/)
DOI: http://dx.doi.org/10.22159/ijap.2018v10i4.25682
INTRODUCTION
Methods for active compound analysis have developed rapidly,
especially since the invention of various analytical instruments such
as HPLC and gas chromatography. The development of quantitative
analysis is driven by the need of more rapid, accurate and simple
method of analysis. On the other side, the efficiency of cost should be
considered; beside the realized of green pharmacy which is strong
issued and recommended to be supported [1-3]. One of the
developing methods prospectively is the determination level of an
active substance by using FTIR instrument due to its free solvent
usage. FTIR method has been developed and reported as a method of
quantitative analysis for some active substances [4-7]. This method
was explained to offer some advantages, such as simple sample
preparation and minimum usage of organic solvents.
Diclofenac sodium is a nonsteroidal anti-inflammation drug (NSAID)
with a mechanism of action inhibiting the cyclooxygenase enzyme,
causing decreasing of prostaglandin synthesis [8, 9]. For some
purposes, the diclofenac tablets are formulated in the coated form,
such as for extended release or protect from degradation [10-15].
Film coating of tablets and other solid dosage also formulated to
mask the unpleasant taste and odours. Furthermore, coated tablet is
produced to improve the appearance of dosage forms; for ease of
swallowing; to achieve colonic drug delivery and controlled drug
delivery, among others. Many excipient are added to be the coating
materials for pharmaceutical products [10-15].
Assay method for diclofenac sodium coated tablet preparation in the
compendia is by using HPLC [8, 9, 16]. Some developments also have
been reported to improve the performance [17-19]. One of the
difficulties in the coated-dosage form analysis is the matrix's
separation. In the common analysis, the matrices are extraction by
appropriate solvents, if needed also supported by other steps of
chromatography. In some practical cases, the coating excipient is
not separated. It will increase the viscosity of the analyte
solution. Then, that causes troubles of the instrument. Besides,
prolongs the time consumption. Another method which has
reported to quantify diclofenac is spectro-photometry UV/visible
[20, 21], and voltammetry-GC [22]. However these methods also
need solvent for extraction
In this study, FTIR instrument was proposed as a quantitative
method for coated tablet of diclofenac sodium directly without
extraction. Diclofenac sodium formula is C14H10Cl2NNaO2 with
molecular weight of 318.129 g/mol. Diclofenac sodium structure as
shown in fig. 1 has amine bond (N-H), carbonyl bond (C = O), and
carbon double bond (C = C) which showing strong peaks in the IR
spectrum [8, 9, 16, 23-25]. These bonds are predicted to have a
correlation with the quantity of the measured substance so that it is
potentially used to determine diclofenac sodium content in a sample.
Fig. 1: Diclofenac sodium chemical structure
The purpose of this study was to develop a more rapid and simple
assay method for diclofenac sodium in the coated tablet using FTIR
directly. It means, without extraction and separation physically.
Furthermore, the parameters of validation resulted would be
compared with the trial obtained by method from the compendia,
completely with a short cost analysis.
MATERIALS AND METHODS
Material
The materials used in this study were: standard of diclofenac sodium
(PT Pharos), KBr crystals (IR-spectra grade), acetone (Brataco,
Indonesia), aqua-bidestilata, methanol pro HPLC, phosphate buffer
pH 2.5, tablet matrix base, micropore 0.45 μm filter paper, and
diclofenac sodium coated tablet preparations as samples.
International Journal of Applied Pharmaceutics
ISSN- 0975-7058 Vol 10, Issue 4, 2018