RP-HPLC Method Development and Validation of Zaltoprofen in Pure Form and in Pharmaceutical Formulation

Boovizhikannan Thangabalan1,2* and Palanirajan Vijayaraj Kumar3
  1. Department of Pharmaceutical Analysis, Southern Institute of Medical Sciences, College of Pharmacy, Mangaldas Nagar, Guntur-522 001, Andhra Pradesh, India
  2. Department of Sciences and Technology, Jawaharlal Nehru Technological University, Hyderabad, Kukatpally, Hyderabad - 500 085, Andhra Pradesh, India.
  3. Faculty of Pharmaceutical sciences, School of pharmacy, UCSI (University college of Sadaya International) University, Malaysia
Corresponding Author: Boovizhikannan Thangabalan, E-Mail : [email protected]
Received:24 September 2012 Accepted: 11 October 2012
Citation: Boovizhikannan Thangabalan* and Palanirajan Vijayaraj Kumar “RP-HPLC Method Development and Validation of Zaltoprofen in Pure Form and in Pharmaceutical Formulation” Int. J. Drug Dev. & Res., October- December 2012, 4(4): 275-278. doi: doi number
Copyright: © 2010 IJDDR, Boovizhikannan Thangabalan et al. This is an open access paper distributed under the copyright agreement with Serials Publication, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.
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Abstract

A simple, rapid, sensitive and precise RP-HPLC method has been developed for the estimation of zaltoprofen in tablet dosage form. In this method Phenomenax Luna C18, 250 x 4.6 mm, 5mm column with mobile phase consisting of acetonitrile and 0.02 M phosphate buffer in the ratio of 50:50 v/v in isocratic mode was used. The detection wavelength is 232 nm and the flow rate is 1.2 mL/min. The method is linear in the concentration range of 20-120 μg/mL. The linearity of zaltoprofen shows a correlation coefficient of 0.999. The percentage recovery ranges from 99.82-100.46 %. The proposed method was validated by determining linearity, accuracy, precision, specificity, LOD and LOQ.

Keywords

Zaltoprofen, RP-HPLC, Validation

INTRODUCTION

Zaltoprofen, 2 - (10, 11 – dihydro – 10 – oxodibenzo [b, f] thiepin – 2 - yl) pro-pionic acid is a potent nonsteroidal anti-inflammatory drug (NSAID) [1]. It is a preferential COX-2 inhibitor, exhibited a potent inhibitory action on the nociceptive responses induced by a retrograde infusion of bradykinin into the right common carotid artery in rats [2]. The drug can be estimated by HPLC in plasma [3-7]. There is a chiral HPLC method for enantioselective analysis [8], Stability-Indicating LC method in bulk drug and formulations [9] and a spectrophotometric method [10]. The present work aims to develop a simple sensitive, precise and accurate RP-HPLC method for the determination of zaltoprofen in pure form and in tablets.

EXPERIMENTAL

Instrumentation

Waters 2695 HPLC system equipped with Phenomenax Luna C18, 250 x 4.6 mm, 5μm column, Rheodyne injector with 10 μL loop, 2996 PDA detector and Empower-2 software was used.

Reagents and chemicals

Pottasium dihydrogenorthophosphate of analytical grade, HPLC grade milli-Q water and acetonitrile were used. Zaltoprofen was a gift sample from Baif Laboratories Ltd. India. The tablets of Zaltoprofen were obtained from local pharmacy.

Preparation of buffer

1.36 gm of potasium dihydrogen orthophosphate was weighed accurately and dissolved in 500 ml of HPLC grade water and pH was adjusted to 5.5 by orthophosphoric acid solution.

Chromatographic conditions

The separation was carried out by Phenomenax Luna C18, 250 x 4.6 mm, 5mm column with the solvent system (mixture of 0.02 M phosphate buffer and acetonitrile in the ratio of 50:50 % v/v) at 30°C. The flow rate was maintained at 1.2 ml/min. The column outlet was monitored at 232 nm. The injection volume was 10 mL and run time was 10 min

Preparation of Standard solution

Pure zaltoprofen (100 mg) was weighed accurately and transferred in to a clean 100 mL volumetric flask. The content was dissolved by using HPLC grade methanol (70 ml), after complete dissolution the volume was made up to the mark by using the HPLC grade methanol which gives 1000 μg/mL of the zaltoprofen.

Linearity

The standard zaltoprofen solution was further diluted in 10 mL volumetric flask to get various concentrations ranging from 20 to 120 μg/mL of drug using mobile phase. From this each calibration standard solutions 10 mL was injected in to the HPLC system. The chromatograms were recorded. The concentration of the zaltoprofen (μg/mL) is taken in X axis and peak area of various standard solutions was taken in Y axis. The linearity graph was plotted.

Estimation in pharmaceutical formulation

Twenty tablets (zaltoprofen) weighed accurately; average weight was calculated and crushed to get fine powder. Powder equivalent to 80 mg of zaltoprofen was weighed accurately and transferred into a 100 mL volumetric flask containing little amount of mobile phase and sonicated for 20 min for complete dissolution of drug. The volume was made up to 100 mL with mobile phase and the solution was filtered through 0.45 μm membrane filter. The solution was suitably diluted with mobile phase to produce suitable concentration and analysed by injecting six times into the HPLC system. The peak area was recorded and amount in tablets estimated from linearity graph.

RESULTS AND DISCUSSION

The system suitability studies were carried out to determine column efficiency, retention time, peak area of single standard solution and peak asymmetry (Table 1). The drug was eluted at 3.7 min and a typical chromatogram for standard is in figure 1. Typical chromatograms for blank and sample are in figure 2 and 3 respectively. The concentration range from 20-120 μg/mL of drug the method showed linear response with the correlation value of 0.999 (Table 2). The accuracy of the method was determined by recovery studies; the percentage of recovery was calculated and the result shows (Table 3) that the method has no interference from the additives used for the formulation. The precision of the developed method was confirmed by performing inter day and intraday assay, %RSD was calculated (Table 3). The developed method was applied to estimate zaltoprofen from the pharmaceutical formulation and assay results are shown in table 3.The limit of detection (LOD) and the limit of quantification (LOQ) were 0.1864 μg/mL and 0.5649 μg/mL respectively.

CONCLUSION

The proposed HPLC method is simple, selective, accurate, precise, linear and rapid. Hence this method can be applied for the quality control of zaltoprofen in pure as well as in pharmaceutical preparations.

ACKNOWLEDGEMENT

The authors express their sincere thanks to Spectrum Pharma Research Solutions, Hyderabad and the management, SIMS College of pharmacy, Guntur for providing the necessary facilities to carry out the research work.

Tables at a glance

Table icon Table icon Table icon
Table 1 Table 2 Table 3
 

Figures at a glance

Figure 1 Figure 2 Figure 3
Figure 1 Figure 2 Figure 3
 

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