UV Spectrophotometric Method for the Estimation of Roflumilast in
Human Serum
Raveendra BG
1*
, Kiran SSB
2
, Kumari VM
2
, Jyothi RK
2
and Bhavani DM
3
1
AKRG College of Pharmacy, Nallajerla-534112, Andhra Pradesh, India
2
OTPR Institute, J N T U, Ananthapuramu-515002, Andhra Pradesh, India
3
DCRMP College, Inkollu-532167, Andhra Pradesh, India
*Corresponding author: Raveendra BG, Department of Pharmaceutical Analysis and Quality Assurance, Nallajerla, Tel: + 919030102494; E-mail:
upendragudimitla@gmail.com
Received date: May 17, 2016; Accepted date: Jun 28, 2016; Published date: Jun 30, 2016
Copyright: © 2016 Raveendra BG, et al. This is an open-access article distributed under the terms of the Creative Commons Attribution License, which permits
unrestricted use, distribution, and reproduction in any medium, provided the original author and source are credited.
Abstract
Ultra violet spectrophotometric method for the estimation roflumilast in spiked human serium. The present study
was spectrophotometric estimation of roflumilast in spiked human serum is based on measurement at the maximum
wavelength 248 nm using 0.2M Hcl as a solvent. The roflumilast stock solution was prepared with distilled water to
produse calibration curve. The standard solution of roflumilast shows absorption maxima at 248 nm. The roflumilast
obeyed beer lamberts law in the concentration range of 40-88µg/ml with regression 0.9987 at 248nm. The overall
percentage recovery of roflumilast was found to be 99.52% which reflects that the method was free from the
interference. The % RSD values of intra day and inter day precision was found to be 0.031 and 0. 046%
respectively, which is less than 2 and hence this method is precise. The values of LOD and LOQ were found to be
0.783 and 2.375 µg/ml, respectively and it indicates this method was sensitive.
Keywords: Serum; Rofumilast; Method development;
Spectrophotometric
Introduction
Rofumilast (Figure 1) is a chemically3-(cyclopropylmethoxy)-N-
(3,5-dichloropyridin-4-yl)-4-(difuoromethoxy) benzamide and it is a
selective, long acting phosphodiesterase-4 inhibitor.
Figure 1: Chemical structure of rofumilast.
Rofumilast was used for the treatment of chronic obstractive
pulmonary disease [1,2] and rofumilast was freely soluble in methanol
and lower alcohols. A few spectrophotometric [3-5] and HPLC [6,7]
methods were reported earlier for the estimation of rofumilast in bulk
and pharmaceutical dosage forms and this method was validated as
per ICH guidelines [8]. Although no method was reported for the
estimation of rofumilast in serum in pharmaceutical dosage forms.
Te present study was authors reported a simple, sensitive, accurate
and precise for estimation of rofumilast in spiked human serum by
using UV spectroscopy.
Experimental
Instrument
ElicoSL164 UV-Visible spectrophotometer with double beam
detector confguration. Te above instruments had automatic
wavelength accuracy 0.1nm and matched quartz cells and Weighing
balance (Elico, India).
Materials
Blank human serum, Rofumilast sample (99.90% purity) was
purchased from Spectrum Pharma Research Solutions, Hyderabad,
India. Hydrochloiric acid and water (HPLC grade) obtained from
Qualigens Fine Chemicals, Mumbai, India.
Method development
Preparation of standard solution: A standard stock solution was
prepared by accurately weighed 1000 mg of rofumilast in 1000ml of
volumetric fask and dissolved in 0.2M of Hcl to obtain a concentration
1000 µg/ml. Further diluting 2.5ml of stock solution to 25ml with
distilled water to get desired concentration of 25µg/ml. Further
diluting 0.4ml of stock solution to 100ml with distilled water to get
desired concentration of 40µg/ml.
Selection of wavelength for analysis of Rofumilast: Accurately
measured 0.4ml of standard stock-III was transferred in to 100ml
volumetric fask and diluted to 100ml to give concentration of 40µg/ml
and it was used for initial spectral scan in the range of 200-400 nm to
detect maximum wavelength and further dilutions for linearity was
Raveendra BG et al., Pharm Anal Acta 2016, 7:6
DOI: 10.4172/2153-2435.1000487
Research Article Open Access
Pharm Anal Acta
ISSN:2153-2435 PAA an open access journal
Volume 7 • Issue 6 • 1000487
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ISSN: 2153-2435
Pharmaceutica Analytica Acta