Research J. Pharm. and Tech. 1(4): Oct.-Dec.

2008,
,

ISSN 0974-3618 www.rjptonline.org

RESEARCH ARTICLE

Validated Spectroscopic Method for Estimation of Aceclofenac from Tablet

Formulation
Rohit Shah*, Chandrakant Magdum, Shital Kumar Patil, Dhanya Kumar Chougule and Nilofar Naikwade

Appasaheb Birnale College of Pharmacy, Sangli South Shivajinagar, Sangli – 416416. Maharashtra
*Corresponding Author E-mail: rohitrshah@yahoo.co.in

ABSTRACT:
Aceclofenac is a non steroidal anti-inflammatory drug with good analgesic and anti-rheumatic properties. Various
methods for analysis of the same are available but are time consuming and expensive. Here we have developed a new,
precise and simple UV spectrophotometric method for estimation of aceclofenac from tablet formulation. The drug
obeyed the Beer’s law and showed good correlation. It showed absorption maxima at 273 nm; in phosphate buffer pH 7.4.
The linearity was observed between 0 – 20 mcg/mL. The results of analysis were validated by recovery studies. The
recovery was more than 99%. The method was found to be simple, accurate, precise, economical and robust.

KEY WORDS: Aceclofenac, UV–Vis Spectrophotometry, Recovery

INTRODUCTION: MATERIALS AND METHODS:

Aceclofenac is a non steroidal anti-inflammatory drug
with good analgesic and anti-rheumatic properties1.
Chemically it is [[[2-[(2, 6-Dichlorophenyl) amino]
phenyl] acetyl] oxy] acetic acid. It is used in various
pain conditions like rheumatoid arthritis, osteoarthritis
and ankylosing spondylatis.1, 2, 3, 4
It is official in British Pharmacopoeia.4 Several
analytical techniques like titrimetric4,5, colourimetric7,
spectroflurimetric7, densitometric8,9, HPLC9-11, RP–
HPLC12,13, spectrophotometric14,15 and stripping
voltametric16 have been reported for assay of
Aceclofenac. However some of these methods are
costlier and time consuming. To overcome these
difficulties spectrophotometric analysis serves to be the
quickest, promising and reliable method for routine
analytical needs.
The aim of the present study is to develop a new
simple, rapid, reliable and precise UV
spectrophotometric method for analysis of aceclofenac
from tablet formulation; method is based on
measurement of UV absorbance of aceclofenac in
phosphate buffer pH 7.4.
Instrument Used
A. Jasco UV-Vis Spectrophotometer Model V – 550 with,
• Spectral bandwidth of 1 nm
• Wavelength accuracy 0.1 nm
B. Bath Sonicator
Reagents and Solution:
All the reagents used in this assay were of analytical grade
and the reagent solutions were prepared using double
distilled water.Aceclofenac pure drug was obtained as a gift
sample from Aarti Drugs Limited, Pune. Tablets of
Aceclofenac were purchased from local market for analysis.
Phosphate buffer pH 7.4 (PBS) was used as a dissolution
medium for the assay.
EXPERIMENTAL:
Determination of λmax:
Weighed amount of Aceclofenac was dissolved in PBS to
obtain a 1000mcg/mL solution. This solution was subjected
to scanning between 200 – 400 nm and absorption
maximum was determined. The effect of dilution on
absorption maxima was studied by diluting the above
solution to 20mcg/mL and scanned from 200 – 400nm.

Standard Stock Solution:

A stock solution containing 1 mg/mL of pure drug was
prepared by dissolving 50mg of Aceclofenac in sufficient
Received on 14.08.2008 Modified on 22.08.2008 PBS to produce 50 mL solution in a volumetric flask.
Accepted on 10.10.2008 © RJPT All right reserved
Research J. Pharm. and Tech. 1(4): Oct.-Dec. 2008;Page 430-432

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Table No. I: Optical characteristics and precision analyst, and time of study. The analysis was performed on
Absorption maxima 273 nm UV-Vis Spectrophotometer model Jasco V-550 and
Beer's law limit 0 – 20 mcg/mL Systronics – 119. Interday and intraday analysis was
Coefficient of Correlation 0.999809 performed by changing the analyst.
Regression equation Y = 0.025052 X + 0.025141
Slope 0.025052 Fig. 1: UV Scan of Aceclofenac in PBS
y intercept 0.025141
Molar absorptivity
8873.512992
(lit/mole/cm)
Sandell's sensitivity
0.039917
(mcg/Sq.cm/0.001)
% COV 0.011869
Confidence limit with 0.05 level 0.00038

Working standard solution:

10 mL of the stock solution was further diluted to 100
mL with PBS to obtain a working standard solution
containing 100mcg/mL.

Linearity and Calibration:

The aliquots working standard solution was diluted
serially with sufficient PBS to obtain the concentration
range of 10 – 100 mcg/mL. A calibration curve for
aceclofenac was obtained by measuring the absorbance
at the λmax of 273 nm. Statistical parameters like the
slope, intercept, coefficient of correlation, standard
deviation, Relative standard deviation, and error were
determined.
Assay:
Accurately weighed the 20 tablets and powdered. The
powder equivalent to 100mg of aceclofenac was
transferred to 100mL volumetric flask and made the
volume to mark with PBS. This mixture was sonicated
in bath sonicator for 45 minutes and filtered through
Whatmann filter paper No. 41. Transferred 5 mL of the
filtrate into a 50 mL volumetric flask and made the
volume to mark with PBS. Aliquots of the sample were
removed and diluted to 10 mL with PBS to obtain
strengths as 20mcg/mL, 40mcg/mL and 60mcg/mL and
determined the respective absorbance at 273nm against
the PBS as blank. Three different formulations of
different manufacturers were used for study.
RESULTS:
The UV scan of standard solution between 200 – 400 nm
showed the absorption maxima at 273nm, shown in fig. 1.
The Beer’s law was verified from the calibration curve by
plotting a graph of concentration vs absorbance. The plot is
shown in fig. 2.
Regression analysis showed very good correlation. The
calibration plot revealed zero intercept which is clear by the
regression analysis equation Y = mX + C. (Where Y is
absorbance, m is the slope and X is the concentration of
aceclofenac in mcg/mL) as obtained by the least square
method. The results thus obtained are depicted in Table No.
I. The results of analysis for assay and recovery studies for
three different formulations were studied and are shown in
Table No. II.
No significant variations were observed on interday and
intraday analysis. Also no significant variations were
observed on changing the instrument make and model.

Recovery studies: Fig. 2 : Calibration curve of Aceclofenac in Phosphate

Recovery studies were performed to judge the accuracy Buffer Solution pH 7.4
of the method. 1mL of standard formulation
(100mcg/mL) was taken in three 10mL volumetric
flask and to it added 1mL, 2mL and 3mL of working
standard solution (100mcg/mL) respectively and made
the volume to mark. The respective absorbance at
273nm was recorded against the blank. The amount of
added concentration was determined from the
absorbance values obtained and percent recovery was
determined for each formulation.

Robustness:
The evaluation of robustness was performed for system
suitability to ensure the validity of analytical
procedure. This was done by varying the instrument,
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Table No. II: Results of analysis
Label % Label Standard Coefficient Standard %
Formulation
Claim Claim found Deviation of Variation error Recovery
T–I 100 mg 101.0481 0.2905 0.2875 0.1677 99.01302
T – II 100 mg 100.9295 0.2565 0.2541 0.1481 99.01297
T – III 100 mg 102.0870 0.1037 0.1016 0.0599 99.05288

DISCUSSION:
The spectrum of aceclofenac in PBS showed the
absorption maxima at 273 nm. No effect of dilution
was observed on the maxima, which confirmed the
maxima at 273nm.
The statistical analysis of data obtained for the
calibration curve of aceclofenac in pure solution
indicated a high level of precision for the proposed
method, as evidenced by low value of coefficient of
variation. The coefficient of correlation was highly
significant. The linearity range was observed between
0 – 20 mcg/mL. The plot clearly showed a straight line
passing through origin (Y = 0.025052 X + 0.025141).
The assay method was validated by low values of %
RSD and standard error, indicating accuracy and
precision of the methods. Excellent recovery studies
further proves the accuracy of the method.
Robustness of the method was studied by varying the
instrument, time of study and analyst. Reproducibility
of the results confirmed the robustness of the method.
CONCLUSIONS:
From the results and discussion the method described
in this paper for the determination of aceclofenac from
tablet formulation is simple, accurate, sensitive and
reproducible. The proposed method utilizes
inexpensive solvents. The proposed method could be
applied for routine analysis in quality control
laboratories.
ACKNOWLEDGEMENTS:
Authors are grateful to Aarti Drugs Limited, Pune for
providing the gift sample of Aceclofenac. We are also
thankful to the Principal and Management of
Appasaheb Birnale College of Pharmacy, Sangli for
providing the necessary facilities to carry out this work.
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