Spectrophotometric Estimation of Mesalazine in Tablet Dosage Form

Asian J. Research Chem. 1(2): Oct.-Dec. 2008,,ISSN 0974-4169www.ajrconline.orgRESEARCH ARTICLESpectrophotometric Estimation of Mesalazine in Tablet Dosage FormPrakash A 1 *, Lone KD 1 , Shukla A 2 , Mandloi R 1 and Ghosh V 1 .1 Dr. D. Y. Patil Institute of Pharmaceutical Sciences and Research Pimpri, Pune-18, Maharashtra, India.2 Sidhhi Vinayaka Institute of Technology and Sciences, Bilaspur*Corresponding Author E-mail: anand_pharma2008@rediffmil.comABSTRACTThree simple, precise and economical UV methods have been developed for the estimation of Mesalazine in tablet dosageform. Mesalazine has the absorbance maxima at 303.5 nm (Method A), and in the first order derivative spectra, showedsharp peak at 241.0 nm (Method B). Method C applied was area under curve (AUC) in the wavelength range of 308.5-298.5 nm. Linearity for detector response was observed in the concentration range of 10-50 µg/ml for all three methods.The proposed methods were successfully applied for the determination of Mesalazine in commercial tablet preparation.The results of the analysis were validated statistically and by recovery studies and were found to be satisfactory.KEY WORDS Mesalazine; Absorbance maxima; Derivative spectroscopy; Area under curve.INTRODUCTION:Chemically Mesalazine (MEZ) is 5-amino salicylicacid 1 . It is an anti-inflammatory drug structurally relatedto salicylates and active in inflammatory bowel disease 2 .Tablet formulations containing 250, 400 and 500 mgMEZ are available in the market. Literature surveyrevealed that Mesalazine is estimated by HPLC 3 andmicellar electrokinetic chromatography 4 . No UVspectrophotometric methods have been reported forestimation of MEZ in single component formulation.Hence, an attempt has been made to develop new UVmethods for its estimation in pharmaceuticalformulations with good accuracy, simplicity, precisionand economy.MATERIAL AND METHODS:Instrument A double-beam Shimadzu UV-Visiblespectrophotometer, with spectral bandwidth of 2 nm,wavelength accuracy ± 0.5 nm and a pair of 1-cmmatched quartz cells was used to measure absorbance ofthe resulting solution.Materials Standard gift sample of Mesalazine wasprovided by Sarax Pharma Pvt. Ltd., Mumbai.Mesalazine tablets were purchased from local market.0.1N HCl was used as a solvent.Received on 01.12.2008 Modified on 23.12.2008Accepted on 25.12.2008 © AJRC All right reservedAsian J. Research Chem. 1(2): Oct.-Dec. 2008; Page 80-82Stock solution: Standard stock solution of MEZ (100 µg/ml)was prepared and used for the analysis.ProcedureMethod A: Absorption Maxima MethodFor the selection of analytical wavelength, 20 µg/ml solutionof MEZ was prepared by appropriate dilution of standardstock solution and scanned in the spectrum mode from 400nm to 200 nm. From the spectra of drug (Fig. 1), λ max ofMEZ, 303.5 nm was selected for the analysis. The calibrationcurve was prepared in the concentration range of 5-40 µg/mlat 303.5 nm. By using the calibration curve, the concentrationof the sample solution can be determined.Method B: First Order Derivative SpectroscopyIn this method, 20 µg/ml solution of MEZ was prepared byappropriate dilution of standard stock solution and scanned inthe spectrum mode from 400 nm to 200 nm. The absorptionspectra thus obtained were derivatized from first to fourthorder. First order derivative spectra were selected for analysisof drug. First order derivative spectra of drug (Fig. 2),showed a sharp peak at 241.0 nm, which was selected for itsquantitation. The calibration curves for MEZ was plotted inthe concentration range of 10-50 µg/ml at wavelength 241.0nm The concentration of the drug present in the mixture wasdetermined against the calibration curve in quantitation mode.Method C: Area Under Curve MethodFor the selection of analytical wavelength, 20 µg/ml solutionof MEZ was prepared by appropriate dilution of standardstock solution and scanned in the spectrum mode from 40080

nm to 200 nm. From the spectra of drugs, area under thecurve in the range of 308.5-298.5 nm was selected forthe analysis. The calibration curve was prepared in theconcentration range of 10-50 µg/ml at their respectiveAUC range. By using the calibration curve, theconcentration of the sample solution can be determined.Asian J. Research Chem. 1(2): Oct.-Dec. 2008,,Linearity: The linearity of measurement was evaluated byanalyzing different concentration of the standard solution ofMEZ. Beer-Lambert’s concentration range was found to be10-50 µg/ml for all three methods.Precision: The reproducibility of the proposed method wasdetermined by performing tablet assay at different timeintervals (morning, afternoon and evening) on same day(Intra-day assay precision) and on three different days (Interdayprecision). Result of intra-day and inter-day precision isexpressed in % RSD. Percent RSD for Intraday assayprecision was found to be 0.0905, 0.0153 and 0.0436 forMethod A, B and C, respectively. Inter-day assay precisionwas found to be 0.0504, 0.0552 and 0.0460 for Method A, Band C, respectively.Fig. 1: Zero order spectra of MesalazineApplication of the proposed method for thedetermination of MEZ in tabletsFor the estimation of drugs in the commercialformulations, twenty tablets were weighed and averageweight was calculated. The tablets were crushed toobtain fine powder. Tablet powder equivalent to 50 mgMEZ was transferred to 100.0 ml volumetric flask andvolume was made up to the mark with 0.1N HCl andultrasonicated for 10 minutes. The solution was thenfiltered through a Whatmann filter paper (No. 41). Thefiltrate was appropriately diluted with 0.1N HCl toobtain 20 µg/ml of MEZ. In Method-A, theconcentration of MEZ was determined by measuring theabsorbance of the sample at 303.5 nm in zero orderspectrum mode. By using the calibration curve, theconcentration of the sample solution can be determined.Method-B, the concentration of MEZ was determined bymeasuring the absorbance of the sample at 241.0 nm, infirst order derivative mode. The results of the tabletanalysis were calculated against the calibration curve inquantitation mode. For Method-C, the concentration ofMSZ was determined by measuring area under curve inthe range of 308.5-298.5 nm. By using the calibrationcurve, the concentration of the sample solution can bedetermined. Results of tablet analysis are shown in TableNo. 1.VALIDATIONThe methods were validated with respect to linearity,accuracy, precision and selectivity.Accuracy: To ascertain the accuracy of proposedmethods, recovery studies were carried out by standardaddition method at three different levels (80%, 100% and120%). Percent recovery for MEZ, by all three methods,was found in the range of 98.33 % to 100.14 %.Fig. 2: First order derivative Spectra of MesalazineTable No. 1: Results of Analysis of Tablet FormulationMethod Label Amountof drug %Label%estimated Claim*ClaimRecovery*(mg/tab) ± S.D.A 400 398.64 99.66 ± 0.2103 99.37B 400 398.74 99.69 ± 0.1791 99.28C 400 399.00 99.75 ± 0.1757 99.47*indicates mean of six determinationsRESULTS AND DISCUSSION:The methods discussed in the present work provide aconvenient and accurate way for analysis of Mesalazine in itspharmaceutical dosage form. Absorbance maxima ofMesalazine at 303.5 nm (Method A); in the first orderderivative spectra, sharp peak at 241 nm (Method B) and areaunder curve in range of 308.5-298.5 nm (Method C) wereselected for the analysis. Linearity for detector response wasobserved in the concentration range of 10-50 µg/ml for allthree methods. Percent label claim for MEZ in tablet analysis,by all the methods, was found in the range of 99.40 % to99.97 %. Standard deviation and coefficient of variance forsix determinations of tablet sample, by all the methods, wasfound to be less than ± 2.0 indicating the precision of themethods. Accuracy of proposed methods was ascertained byrecovery studies and the results are expressed as % recovery.81

Percent recovery for MEZ, by all the methods, wasfound in the range of 98.33 % to 100.14 % values ofstandard deviation and coefficient of variation wassatisfactorily low indicating the accuracy of the methods.Based on the results obtained, it is found that theproposed methods are accurate, precise, reproducibleand economical and can be employed for routine qualitycontrol of Mesalazine in its tablet formulation.ACKNOWLEDGEMENTS:The authors are very thankful to Sarax Pharma Pvt. Ltd.,Mumbai, for providing gift samples of Mesalazine.REFERENCES:1. Budavari S. The Merck Index. Merck Research Lab,Division of Merck and Co., Inc., Whitehouse Station NJ,1996; 12 th ed: pp 1163.2. Tripathi KD. Essentials of Medical Pharmacology. JaypeeBrothers Medical Publishers (P) Ltd, New Delhi. 2004;5th ed: pp 620-621.3. Nobilis M, Vybiralov Z, Sladkova K, Lisa M, HolcapekM and Kvetina J. J Chromatogr A. 2006; 1119(1-2):299-308.4. Gotti R, Pomponio R, Bertucci C and Cavrini V. JChromatogr A. 2001; 916(1-2): 175-183.Asian J. Research Chem. 1(2): Oct.-Dec. 2008,,82