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org | ISSN: 2277 2782


INTERNATIONAL JOURNAL OF NOVEL TRENDS IN PHARMACEUTICAL SCIENCES

RESEARCH ARTICLE

RP-HPLC method development and validation of valizodone


in pure and tablet dosage form
Thangabalan B, Lakshmi Narusu R*, SyedaliFathima SK and ManoharBabu S
SIMS College of Pharmacy, Mangaldas Nagar, Guntur-522 001, India.
Abstract
A simple, precise, rapid, accurate and economic reverse phase high performance liquid chromatographic
method has been developed for the estimation ofValizodone in tablet dosage form. The separation was
achieved by using octadecylsilane column (C 18 ) and acetonitrile : water in proportion of 60:40 v/v as mobile
phase, at a flow rate of 1.0 ml/min. The detection was carried out at 240 nm. The retention time of
Valizodone was found to be 4.3 min. The limit of detection and limit of quantitation were found to be 0.11
g/ml and 0.33 g/ml respectively. The accuracy and reliability of the proposed method was carried out by
evaluating various validation parameters like linearity, precision, accuracy and specificity according to ICH
guidelines.
Key words: Valizodone, HPLC, Validation
INTRODUCTION
Vilazodone is chemically 5-(4-[4-(5-cyano-1H-indol3-yl) butyl] piperazin 1-yl) benzofuran -2carboxamide. It is a strong dopamine antagonist. It
has high affinity for D2 dopaminergic receptors. The
literature survey reveals that the drug can be
estimated by RP-HPLC [1], LCMS [2,3]. The aim of
the study was to develop a simple, precise and
accurate RP-HPLC method for the estimation of
Vilazodone in pure drug and in pharmaceutical
dosage form.
EXPERIMENTAL METHODS
All the reagents used were HPLC grade. HPLC
experiments were performed on a Waters HPLC
system equipped with Phenomenex Luna C18, 5m
(4.6250 mm) column, waters pumps, dual
wavelength UV detector and Empower 2 software
was used. The mobile phase consisted of
acetonitrile: water (60:40, v/v) that was set at a flow
rate of 1 mL/min.
Procedure
Stock solution of Vilazodone was prepared by
dissolving accurately weighed 100 mg of the drug
in 100 mL of mobile phase (final concentration, 1
mg/mL). Calibration plot were constructed by
analysis
of
appropriate
working
solutions
(concentration 10, 50, 100, 150, 200 and 250 g/mL)
of Vilazodone in the mobile phase and plotting
VOLUME 5 | NUMBER 2 | APR | 2015

concentration against peak area response for each


injection. Unknown samples were quantified by
reference to this Beers plot.
Sample analysis
Twenty tablets were weighed and powdered. An
amount of powder equivalent to 100 mg
Vilazodone was accurately weighed and transferred
to a 100 mL volumetric flask. Mobile phase (50 mL)
was added and the mixture was sonicated for 10
min, for complete extraction of the drug, and the
solution was diluted to volume with mobile phase.
The solution was centrifuged at 4000 rpm for 10
min, and the clear supernatant was collected and
filtered through a 0.2 m membrane filter. This
solution was taken and diluted to 10 mL with
mobile phase, to furnish a 100 g/mL solution, of
which 20 L was injected for HPLC analysis.
RESULTS AND DISCUSSION
The retention time of the drug was 4.3 min (figure
1). There was no interference from diluents used
forpreparationoftablets(figure
2).Chromatographicparameters such as peak
asymmetry and capacity factor were found to be
To whom correspondence should be addressed:

Lakshmi Narusu R
Email: chanduvenkat01@gmail.com

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Tekade et al., Formulation and in-vitro evaluation of famotidine bilayer floating tablet

1.03 and 0.921 respectively. The limit of detection


(LOD) and limit of quantification (LOQ) were found
to be 0.11 and 0.33 g/mL respectively.
Analytical recovery studies were carried outfrom a
series of spiked concentrations added to the pre-

analysed dosage form (Table 1). The accuracy of


the method was carried out by adding standard to
preanalysed pharmaceutical formulation at 50, 100
and 150 % levels and report is in Table 2.

Table 1. Determination of Vilazodone in tablets


Sample
Label claim/tablet (mg)
Amount found* (mg/tab)
Vilazodone Tablets
50
49.98
* Mean of 5 determinations
Table 2.Recovery study data of Vilazodone.
Drug
Amount added (g)
Amount recovered (g)
Percentage recovery (%)
50
49.97
99.94
Vilazodone
100
100.06
100.07
150
150.12
100.01
Fig 1. Standard chromatogram of Vilazodone

Analysing five replicates of fixed amount of


Vilazodone enabled checking the precision and
accuracy of the proposed method. The precision of
the method was calculated in terms of the relative
standard deviation.
Low values of relative standard deviation (0.46 %)
and percentage errors at 95% confidence limits
(0.61) indicated high precision and accuracy of the
proposed method. Hence the present method can
be used for the routine analysis of Vilazodone in
formulation.
REFERENCES
1. Parameswara
Reddy
B,
Pramod
N,
Venkateswararao P, Sudhakarbabu AMS.
Method development and validation for the
assay of vilazodone in bulk and formulation by
using RPHPLC technique. International Journal
of Biological &Pharmaceutical Research, 3(6),
2012, 789-795.
2. Kalariya PD, Talluri MV, Patel PN, Srinivas R.
Identification of hydrolytic and isomeric Noxide degradants of vilazodone by on line LCVOLUME 5 | NUMBER 2 | APR | 2015

Fig 2. Sample chromatogram of Vilazodone

CONCLUSION
The developed RP-HPLC method was simple,
sensitive, precise and accurate and hence can be
used in routine for the determination of
Vilazodone in pure as well as pharmaceutical
preparations.
ACKNOWLEDGEMENT
The Authors are thankful to the management SIMS
Group of Institutions, Guntur, for providing
necessary facilities to carry out the research work.

3.

ESI-MS/MS
and
APCI-MS.
Journal
of
Pharmaceutical and Biomedical Analysis, 102,
2015, 353-365.
Zeng LL1, Sun LL, Zou Q, Zhou F, Wei P, Ouyang
PK. Bioavailability comparison of a new form of
vilazodone XVII to IV in beagles using liquid
chromatography/mass
spectrometry.
Biomedical Chromatography, 28(12), 2014,
1738-1743.

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