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Received 21/12/2014
Available online
31/12/2014
Keywords
Mometasone Furoate,
Formoterol Fumarate,
Spectrophotometric Method,
Analysis.
ABSTRACT
Two spectrophotometric methods Zero crossing derivative and ratio- spectra derivative
spectrophotometric methods were developed for the determination of Mometasone furoate
(MF) and Formoterol fumarate (FF) in the pharmaceutical dosage form. Zero crossing
dervative spectrophotometry involves amplitudes measurement of the first derivative spectra
of the standard and sample solution at 267.56 nm for MF and 306 nm for FF. Ratio spectra
derivative spectrophotometry involves amplitudes measurement of the ratio first derivative
spectra at 263nm and 267.30 nm for MF and 293.08 and 302.60 nm for FF. The calibration
graph follows beers law in the range of 30-200 g /ml of MF and 2-6 g /ml for FF. The
accuracy and precision of the method were validated statistically. So it can be a preferable
method for routine analysis due to its simplicity and economical advantages.
Copy right 2014 This is an Open Access article distributed under the terms of the Indo American journal of Pharmaceutical
Research, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.
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Please cite this article in press as Aarti. S. Zanwar et al. Spectroscopic methods for the simultaneous estimation of Mometasone
furoate and Formoterol fumarate in rotacaps. Indo American Journal of Pharm Research.2014:4(12).
5928
Corresponding author
Aarti. S. Zanwar
Department of Pharmacy,
Sumandeep Vidyapeeth, Piparia,
Vadodara-391760,Gujarat
aarti.zanwar @ gmail.com
INTRODUCTION
Nowadays combinational therapy of mometasone fumarate and formoterol furoate has been used in the treatment of COPD
and asthma as it produces the additive effect for improving the symptom, lung function and reduces exacerbation in patient.[1]
Mometasone furoate (MF) (Fig.1) is a highly potent synthetic chlorinated glucocorticosteriod. It is used in the treatment of
glucocorticoid responsive disorders of dermatology, seasonal and perennial allergic rhinitis and asthma. [2]. Formoterol fumarate (Fig
2) appear to be more effective than shorter acting 2-agoinst in the treatment of nocturnal and exercise induced asthma. It acts locally
in the lung as a bronchodilator [3]. Literature survey reveals that serval analytical method have been published for the estimation of
MF alone or in combination with other drugs like fucidic acid, terbinafine HCl, miconazole, eberconazole nitrate etc. Some of these
methods include HPLC, GC, supercritical fluid chromatography and UV spectrophometry[4-11]. Various method has also been
reported for the estimation of FF alone and in combination with other drugs including HPLC, GC, and UV spectrophometry [12-14].
However, no UV method has been reported for the simultaneous estimation of MF and FF in rotacaps by zero crossing derivative and
ratio derivative spectrophotometry method. So, the aim of the present work was to develop simple, sensitive and validated two
spectrophotometric methods for the simultaneous determination of MF and FF in their pharmaceutical preparations.
Experimental work
Instrumentation:
Shimadzu UV-1800 spectrophotometer connected to computer loaded with Shimadzu UV probe 2.10 software was used for
all the spectrophotometeric measurements. All weighing were done on electronic balance( model Ohaus adventurer Pro).
Ultrasonicator was used for sample solution preparation.
Reagents and chemicals:
Analytical pure sample of MF and FF were obtained as a gift sample from Sun Pharma, Vadodara. These sample were used
without further purification. The formulation Evocort manufactured by Cipla was purchased from the local market containing MF
(200g) and FF (6 g) per rotacap. Analytical grade methanol was purchased from Merck Mumbai was used throughout the study.
Preparation of standard solution and calibration curve:
Individual standard stock solution of MF (100 g/ ml) and FF (100 g/ ml) were prepared by dissolving 10 mg of MF and 10
mg of FF in 100 ml methanol in separate volumetric flask. The std stock solution were further diluted separately to obtained working
standard solution of the conc. 30-200 g/ ml of MF and 2-6 g/ ml of FF.
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5929
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Fig.4 Overlain first derivative spectra of MF and FF, for the estimation
of MF when FF spectra is showing zero crossing at 267.56 nm and
for FF when MF is showing zero crossing at 306 nm.
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5930
MF
263
30-200
0.9991
3.382
-0.004
0.07638
0.09018
0.0879
0.266
0.81
1.56
267.3
30-200
0.9994
-3.020
-0.328
0.0503
0.0851
0.0929
0.2817
0.69
1.06
Method RD1
FF
293.08
302.60
2-6
2-6
0.9982
0.9986
0.238
-0.257
0.251
-1.200
0.02685 0.02525
0.01752 0.02163
0.2429
0.0183
0.7361
0.8416
0.89
0.96
1.38
1.32
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Table 2: Recovery analysis for the proposed spectrometric method D1 and RD1 applied to the Rotacaps.
% Recovery of MF
% Recovery of FF
Spike level(%) Method D1
Method RD1
Method D1
Method RD1
267.56nm
263nm
267.3nm
306nm
293.08nm
302.60nm
80
99.24 0.32 99.730.56
99.380.53
98.440.25
99.260.44 98.670.44
100
100.180.47 99.540.68
99.770.50
97.7830.51 98.780.33 99.160.84
120
99.17 0.52 100.10 0.86 100.350.63 98.100.59
98.250.32 99.060.23
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Parameter assessed
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MF
FF
200
6
Method 1
% S.D*(n=6)
100.400.736
98.910.562
Method 2
% S.D*(n=6)
101.20 0.6377
99.200.812
The main advantage of the ratio derivative method is the chance of easy measurement in corresponding to peak so it permits
the use of the wavelength of the highest value of analytical signal. Moreover, the presence of a lot of maxima and minima is another
advantage by the fact that these wavelengths give an opportunity for the determination of active compounds or excipients which
possibly interfere with the analysis. The influence of the and scaling factor for the obtaining the first derivative of the ratio spectra
as well as the effect of divisor concentration on the calibration graphs for the proposed mixture was studied in order to select the best
factors affecting the determination of the analytes. Results indicated that =2 and scaling factor 4 was the most suitable one.
Determination of both drugs was done by dividing the absorption spectra of MF by that of standard spectra of FF (6 g/ml) while the
absorption spectra of FF were divided by that of the standard spectra of MF (30 g/ml).
The proposed methods for the simultaneous estimation of MF and FF in combined dosage form were found to be accurate,
simple and rapid which can be well understood from validation data as given in table (1) &(2). Linearity was observed by linear
regression equation method for MF and FF in different conc. range. The correlation coefficient of these drugs was found to be close to
1.000 indicating good linearity. Percentage RSD for intraday and inter day was found to be less than 2 and the % recovery for both the
drug was found within the range(98.10%-100.18%)as mention in table (2), which indicates the validity of both method. The analysis
results of the rotacaps are given in the table (3).
CONCLUSION
Zero crossing derivative and ratio- spectra derivative spectrophotometric methods were applied successfully for the
simultaneous analysis of MF and FF in the rotacaps. The proposed methods were simple, cost effective, accurate and precise which
can be used for the routine quality control analysis of MF and FF in combined dosage forms.
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ACKNOWLEDGMENT
The authors are thankful to the Research Director , Sumandeep Vidyapeeth for providing all the facility for doing the research work.
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