Original Article
FORMULATION DEVELOPMENT AND EVALUATION OF GASTRO-RETENTIVE DOSAGE FORM
OF ATAZANAVIR SULPHATE
HEMANT K. JAIN
*
, MADHURI TAWARE
Department of Quality Assurance Techniques, Sinhgad College of Pharmacy, Vadgaon (Bk.), Pune 411041, Maharashtra, India
Email: hemantkjain2001@yahoo.co.in
Received: 07 Jul 2017 Revised and Accepted: 22 Nov 2017
ABSTRACT
Objective: To improve dissolution properties of atazanavir sulphate by preparing gastro-retentive granules by solid dispersion method and
development of RP-HPLC method for estimation of this drug.
Methods: Estimation of atazanavir sulphate was done using high performance liquid chromatography (HPLC) on inertsil column (5 µm, 250x4, 6
mm) with a mobile phase consists of methanol: water (91:9 v/v), at 0.5 ml/min flow rate and 249 nm UV detection. The method was validated as
per ICH guidelines. Selection of the carrier for gastro-retentive formulation was based on phase solubility study of the drug. Solid dispersions of
gastro-retentive granules of different composition of drug and carrier, were prepared by the kneading, heating and solvent evaporation. A
3
2
factorial design was applied to optimize the gastro-retentive formulation. The amounts of polyethylene glycol 6000 (PEG 6000) (X1) and
hydroxypropyl methyl cellulose (HPMC) (X2) were selected as independent variables and in vitro-release at 5, 9 h and total floating time was
selected as dependent variables.
Results: HPLC method was found to be linear in a concentration range of 10-60 μg/ml of the drug (r
2
= 0.999). The low value of % RSD in precision
study indicates reproducibility of the method. The low value of LOD and LOQ suggests the sensitivity of the method. The solubility enhancement
study of drug with various carriers followed descending order of solubility [Gelucire 44/14>PEG 6000>polyvinyl pyrrilidone (PVP)]. Highest %
cumulative release was observed for the heating method at drug polymer (PEG 6000) ratio 1:5. Hence, this ratio has been selected for preparation
of solid dispersion. From comparison of dissolution profile of formulated batches, formulation F4 [containing PEG6000 (1.6 g) and HPMC (200 mg)]
showed promising dissolution parameters with desired floating properties.
Conclusion: Results obtained by validation studies suggested that the developed HPLC method is simple, accurate, precise and can be used for
routine analysis of atazanavir sulphate formulation. Results of evaluation of prepared batches indicate that batch F4 is a promising formulation for
gastro-retentive dosage form of drug.
Keywords: Atazanavir sulphate, Formulation development, Gastro-retentive dosage form, Floating granules, RP-HPLC, Validation
© 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/ijpps.2018v10i1.21179
INTRODUCTION
Approx. 35 million people were died from acquired immuno
deficiency syndrome (AIDS) related illnesses since start of the
epidemic and about 36.7 million people were living with human
immunodeficiency virus (HIV) infection during December 2015
throughout the world. The number of HIV infected patients is
increasing every year [1]. In this context, an effective drug therapy is
needed for the treatment of this infection. Atazanavir sulphate is a
novel azapeptide HIV protease inhibitor with high specificity which
prevents multiplication of HIV [2]. Atazanavir sulphate is chemically
(3S,8S,9S,12S)-3,12-bis(1,1-dimethylethyl)-8-hydroxy-4,11-dioxo-9-
(phenylmethyl)-6-[[4-(2-pyridinyl)phenyl]methyl]-2,5,6,10,13-penta
azatetradecanedioic acid dimethyl ester, sulphate (1:1) [3].
Atazanavir sulphate is an antiretroviral drug which belongs to BCS
class-2 drugs, associated with poor solubility. Atazanavir sulphate
has less bioavailability due to pH-dependent solubility and
absorption [4, 5].
Therefore, there is need to increase the solubility of this drug. Various
techniques are used for solubility enhancement of poorly soluble drugs
[6, 7]. Solid dispersion method has been selected in this project for
solubility enhancement by preparing pH dependent floating granules.
Some methods have been reported for determination of atazanavir
sulphate by HPLC [8-12]. In order to reduce the cost of analysis an
economical HPLC method has been developed. This paper presents
formulation development of gastro-retentive granules of atazanavir
sulphate as well as development and validation of RP-HPLC method
for estimation of this drug.
Fig. 1: Chemical structure of atazanavir sulphate
International Journal of Pharmacy and Pharmaceutical Sciences
ISSN- 0975-1491 Vol 10, Issue 1, 2018