Original Article
LIQUID CHROMATOGRAPHIC QUANTIFICATION OF TERNARY MIXTURE OF ANTI-VIRAL
DRUGS AND APPLICATION TO ASSESSMENT OF THEIR TABLET DOSAGE FORM
ANUMOLU P. D., ANUSHA K., MRUDULA KIRAN A., MONIKA P., SOWNDARYA NSKR, SUNITHA G.*
Gokaraju Rangaraju College of Pharmacy, Department of Pharmaceutical Analysis and Quality Assurance, Osmania University, Hyderabad
500090, Telangana state, India
Email: g.sunitha88@gmail.com
Received: 17 Apr 2015 Revised and Accepted: 25 Nov 2015
ABSTRACT
Objective: To establish a validated liquid chromatographic method for the quantification of Tenfovir disoproxil fumarate (TENO), Lamivudine
(LAM) and Nevirapine (NEV) in ternary combination and in its tablet dosage form.
Methods: The three drugs were well resolved using ODS C18
Results: The response was a linear function of analyte concentration over the concentration range of 45-105 µg/ml for tenofovir disoproxil
fumarate, lamivudine and between 30-70 µg/ml for nevirapine with a correlation coefficient>0.9997. The % RSD values of precision and accuracy
studies were found to be less than 2.
column (250 x 4.6 mm, 5μm) with a mobile phase consisting of phosphate buffer, pH 3.0-
acetonitrile (60:40, v/v) with a flow rate of 1.0 ml/min at UV detection wavelength 252 nm. The developed method was validated as per ICH guidelines.
Conclusion: The proposed method was validated as per standard guidelines. The results obtained from assay values were in good agreement with
the labeled amount of the marketed tablet dosage form RICOVIR-LN. The method holds promise for routine quality control of this ternary
combination in bulk and pharmaceutical formulations.
Keywords: Column liquid chromatography, Tenofovir Disoproxil Fumarate, Lamivudine, Nevirapine.
© 2016 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/ )
INTRODUCTION
Tenofovir chemically designated as {[(2R)-1-(6-amino-9H-purin-9-yl)
propan-2-yl) oxy] methyl} phosphonic acid, is an anti-retroviral agent
currently used in the treatment of HIV. Its mechanism of action involves
the inhibition of HIV reverse transcriptase activity by competing with
natural substrate deoxyadenosine5’-triphosphate by DNA chain
termination. Nevirapine is chemically designated as 2-cyclopropyl-7-
methyl- 2,4,9,15-tetra aza tricyclo [9.4.0.0^{3,8}] pentadeca-
1(15)3,5,7,11,13-hexane-10-one, is an antiretroviral agent used in HIV
treatment. Its mechanism of action involves binding of reverse
transcriptase directly and blocks RNA-dependent and DNA–dependent
polymerase activities by causing disruption of enzyme catalytic site.
Lamivudine is also an anti-retroviral agent which is chemically
designated as 4-amino-1-[(2R, 5S)-2-(hydromethyl)-1,3-oxathiolan-5-
yl]-1,2-dihydropyrimidin-2-one, used in the treatment of HIV. Chemical
structures of these drugs were shown in fig.-1. The combination of three
drugs used for the treatment of HIV as a ternary combination [1-2].
Fig. 1: Chemical structures of tenofovir disoproxil fumarate (A),
Nevirapine (B) and Lamivudine (C)
An all-embracing literature search revealed that only one analytical
method using high-performance liquid chromatography has been
previously reported for the determination of this combination by
gradient elution [3]. Few analytical methods based on HPLC, HPTLC,
UV spectroscopy are available for the determination of these drugs
individually and in combination with other drugs in different dosage
forms, but there is no isocratic HPLC method for simultaneous
quantification of three drugs in combined dosage form [4-14].
Keeping this point into consideration, present investigation has been
undertaken with the objective to develop and validate simple
isocratic RP-HPLC method for evaluation of this tertiary
combination of drugs in bulk and tablet dosage form.
MATERIALS AND METHODS
Instrument and chromatographic conditions
The ternary combination of three drugs were well separated by using
a Shimadzu model LC-20AD HPLC system connected to LC solutions
software, equipped with an SPD-20A prominence UV detector and
ODS, C18
Chemicals and reagents
column (250x4.6 mm, 5 µm) maintained at 25ºC. Isocratic
elution was performed using acetonitrile and phosphate buffer, pH 3.0
(40:60, v/v) with flow rate 1.0 ml/min at UV detection wavelength
252 nm. 20 µl of sample was injected into the HPLC system.
Tenofovir disoproxil fumarate, nevirapine and lamivudine standards
and tablet dosage forms were obtained from Mylan laboratories
(Hyderabad, India). Milli-Q-water was used throughout the
experiment. Acetonitrile and methanol (HPLC grade), sodium
hydroxide, potassium dihydrogen phosphate, orthophosphoric acid
were purchased from Merck (Mumbai, India).
Preparation of standard stock solution
The standard stock solution was prepared by dissolving 75 mg of
tenofovir diisopropyl fumarate, 50 mg of nevirapine and 75 mg of
lamivudine in 100 ml of mobile phase to get concentrations of 750
µg/ml, 500 µg/ml and 750 µg/ml respectively. This stock solution
was further diluted with mobile phase to get the required
concentration of drugs. Solutions were filtered through 0.22 µm
membrane filter prior to injection into HPLC system.
Assay of commercial tablets
Twenty tablets of RICOVIR-LN were purchased, weighed and
crushed into fine powder. An accurately weighed portion of tablet
powder equivalent to 75 mg, 50 mg and 75 mg of tenofovir
International Journal of Pharmacy and Pharmaceutical Sciences
ISSN- 0975-1491 Vol 8, Issue 1, 2016