T. Nuzhath et al, JPBMAL, 2015, 3(2): 273–277

ISSN: 2347-4742

Journal of Pharmaceutical and Biomedical Analysis Letters Journal Home Page: www.pharmaresearchlibrary.com/jpbmal

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Development and Validation for the Extractive Colorimetric Methods for the Determination of Sumatriptan Succinate in Bulk and its Tablet Dosage Form T. Nuzhath*, S. Muneer, B. Mohammed Ishaq, Dr. Hindustan Abdul Ahad, B. Famida, S. Parveen Department of Pharmaceutical Analysis, Balaji College of Pharmacy, Rudrampeta Bypass, Anantapur515001, AP, India ABSTRACT Two simple, rapid, accurate, precise and economic spectrophotometric methods have been developed for the estimation of Sumatriptan Succinate in pharmaceutical formulation. These methods are based on the formation of chloroform soluble ionassociation complexes of Sumatriptan Succinate with bromocresol green in a phosphate buffer of pH 3.6 (Method I) and with bromothymol blue in a phosphate buffer of pH 3.6 (Method II). This property of the drug was followed for the development of colorimetric methods for analysis of drug. The complex of with bromocresol green and bromothymol blue showed λmax at 418 nm and 413 nm, respectively. The absorbance was found to increase linearly with increasing concentration of Sumatriptan Succinate with correlation coefficient values (0.999), for both method I and II. The systems obeyed the beer law in the range of 10-200 μg/ml for bromocresol green and bromothymol blue, respectively. Recovery studies showed satisfactory results indicating that none of common additives and excipients interferes with the assay method. Various analytical parameters were evaluated and found satisfactory. The proposed methods are found to be simple, sensitive, accurate, precise and economic, can be successfully applied for the analysis of Sumatriptan Succinatein pharmaceutical dosage form. Keywords: Sumatriptan Succinate (SUM), Bromocresol green (BCG), Bromothymol Blue (BTB), Colorimetric analysis, Extractive spectrophotometry, Distilled water,

ARTICLE INFO CONTENTS 1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .274 2. Materials and Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .274 3. Results and discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .275 4. Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . .276 5. Acknowledgement. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . .276 6. References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 276 Article History: Received 25 May 2015, Accepted 24 June 2015, Available Online 18 July 2015 *Corresponding Author

T. Nuzhath Department of Pharmaceutical Analysis, Balaji College of Pharmacy, Rudrampeta Bypass, Anantapur–515001, AP, India Manuscript ID: JPBMAL2602

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Citation: T. Nuzhath, et al. Development and Validation for the Extractive Colorimetric Methods for the Determination of Sumatriptan Succinate in Bulk and its Tablet Dosage Form. J. Pharm, Biomed. A. Lett., 2015, 3(2): 273-277. Journal of Pharmaceutical and Biomedical Analysis Letters

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T. Nuzhath et al, JPBMAL, 2015, 3(2): 273–277

ISSN: 2347-4742

Copyright © 2015 T. Nuzhath, 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 work is properly cited.

1. Introduction Sumatriptan succinate is a synthetic drug belonging to the triptanclass. Structurally, it is an analog of the naturally occurring neuro-active alkaloids dimethyltryptamine (DMT), bufotenine, and 5-methoxy-dimethyltryptamine, with an N-methyl sulfonamidomethyl group at position C-5 on the indole ring. It is effective for ending the headache of a migraine.1 Literature survey reveals that there are few spectrophotometric methods either individually or in combined dosage forms2-7 and conductometric method 8 were also reported. There was no spectrophotometric method for the estimation of this drug using bromocresol green(BCG) and bromothymol blue(BTB). Therefore in the present study, two extractive spectrophotometric methods for the estimation of SUM in pure and tablet dosage form are described. The methods-I and II are based on the formation of colored ion-pair complex of the drug with BCG and BTB in acetate buffer, respectively.

Figure 1: Chemical structure of Sumatriptan Succinate

2. Materials and Methods Instruments and reagents An analytically pure sample SUMof was kindly gifted by MSN laboratories, Hyderabad, India. Distilled water prepared in-house, was used as solvent. A PG Instrument T60 UV/VIS spectrophotometer was used with 1 cm matched quartz cell. Capsule formulation [Suminat 50, Sun Pharma laboratories ltd, India] was procured from a local pharmacy with labeled amount 50 mg per Tablets. A calibrated digital pH(ELICO, India) meter was used for pH measurements. Chloroform (AR grade, S.D. Fine Chemical Ltd., Mumbai, India), disodium hydrogen phosphate (AR grade, SD Fine Chemical Ltd., India), citric acid (AR grade, S.D. Fine Chemical Ltd., Mumbai, India), bromocresolgreen (AR grade, Fine Chemicals Ltd., India),bromothymol blue (AR grade, Fine Chemicals Ltd., India), sodium hydroxide (ARgrade, S.D. Fine Chemical Ltd., Mumbai, India)and Whatman filter paper no. 41 (Millipore, USA)were used in the study. Preparation of buffer solution (Phosphate buffer, pH 3.6): Disodium hydrogen phosphate (0.09 g) and 0.13 g of citric acid was accurately weighed and dissolved in water (100ml). Preparation of Bromocresol green dye (0.5%) Journal of Pharmaceutical and Biomedical Analysis Letters

Bromocresol green reagent (10 mg) was accurately weighed and transferred to 100 ml volumetric flask, dissolved and diluted with distilled water and made up to mark. Preparation of Bromothymol blue dye (0.5%) Bromothymol blue reagent (10 mg) was accurately weighed and transferred to 100 ml volumetric flask dissolved and diluted with distilled water and made up to mark. Preparation of SUM standard stock solution SUM (100 mg) was accurately weighed and transferred into 100 ml volumetric flask, dissolved and diluted with distilled water to obtain the concentration of 1000 μg/ml. Working standard solution (100 μg/ml) was prepared by diluting standard stock solution (10 ml) to 100 ml with distilled water. Optimization of different conditions Condition under which reaction of SUM with dyes fulfill the essential requirements was investigated. Various conditions like pH and volume of buffer, wavelength of maximum absorbance and stability of dye-drug complex were optimized at room temperature. Validation of the proposed methods: The proposed method was validated according to the International Conference on Harmonization (ICH) guidelines.7 Linearity Method I (BCG Method) Calibration curve was plotted over a concentration range of 10-200 μg/ml for SUM. From the working standard solution, a dilution of 1 ml with 10 ml was made to obtain final concentration 100 μg/ml. The solutions were transferred to a series of separating funnels. Buffer solution (2.0 ml) was added to each separating funnels, 1 ml of BCG was added and shaken well, 5 ml chloroform was added to each and shaken well and kept for few minutes. Later the extracts were taken into 10 ml volumetric flasks using multiple extractions and make up the volume with chloroform, and absorbance of the solution was measured at 418nm against reagent blank. The standard calibration plot of absorbance versus concentration was prepared to calculate the amount of the analyte drug in capsule sample solution. Method II (BTB Method) Calibration curve was plotted over a concentration range of 10-200 μg/ml for SUM. From the working standard solution, a dilution of 1 ml with 10 ml was made to obtain final concentration 100 μg/ml. The solutions were transferred to a series of separating funnels. Buffer solution (2 ml) was added to each separating funnels, 1 ml of BTB solution was added and shaken well,5 ml of chloroform was added to each and shaken well and kept for few minutes. Later the extracts were taken into 10 ml volumetric flasks using multiple extractions and make up the volume with chloroform, and absorbance of the solution was measured at 413 nm. The standard calibration plot of absorbance versus concentration was prepared to calculate the amount of the analytedrug in capsule sample solutions. 274

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Accuracy (%Recovery): The accuracy of the methods was performed by calculating recovery of SUM by the standard addition method. Known amounts of standard solutions of SUM were added at 50, 100 and150% levels to prequantified sample solutions of 100 μg/ml SUM for both BCG and BT methods. Each sample was prepared in triplicate at each level. The amount of SUM was estimated by applying obtained values to regression equation. Method precision (% Repeatability) The precision of the instrument was checked by repeated scanning and the absorbance is measured for solutions of 100 μg/ml (n = 6) with BCG and BTB, respectively without changing the parameters for the method. The repeatability was expressed interms of % relative standard deviation (% RSD)and is reported in Table 1. Limit of detection and Limit of quantification The limit of detection (LOD) and the limit of quantification (LOQ) of the drug was derived by calculating the signal-tonoise ratio (S/N, i.e., 3.3for LOD and 10 for LOQ) using the following equations as per ICH guidelines.7 LOD = 3.3 × SD/Slope LOQ = 10 × SD/Slope Where SD = the standard deviation of the response Determination of SUM in pharmaceutical formulations (Tablets): Twenty Tablets were accurately weighed and average weight was determined. The quantity of the powder equivalent to 100 mg of SUM was transferred to a 100 ml volumetric flask. The content was mixed with diluent (50 ml), sonicated for 5 min. to dissolve drug and the volume was adjusted up to the mark with diluent to give concentration (1000 μg/ml). The solution was then filtered through whatman filter paper no. 41. The above solution (10 ml) was diluted to100 ml with diluent (100μg/ml). An aliquot of this solution was taken and analyzed as described. The amount of SUM present in capsule sample solution was determined by fitting the responses into the respective regression equations for SUM in both the methods.

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the accuracy and reproducibility of the proposed methods, recovery studies were performed. The data obtained by recovery studies indicate noninterference from the excipients used in the formulations. The percentage recoveries were close to 100% and %RSD were within 2%indicate the accuracy of the methods shown in Table 1 respectively. This study revealed that the common excipients and other additives are usually present in the capsule dosage forms do not interfere in the analysis. These developed methods were used for the estimation of SUM from marketed capsule formulations. Optical characteristics and summary of all the validated parameters for both the methods for SUM is reported in Table.1

Figure 2: Spectra of SUM with BCG

3. Results and Discussion The developed methods were based on addition of drug in its ionized form to an ionized dye, BCG and BTB to yield a salt (ion-pair) that was extracted into an organic solvent such as chloroform. The indicator dye was added in excess and the pH of the aqueous solution was adjusted to a value where both the drug and dye were in the ionized forms. This property of the drug was followed for the development of sensitive colorimetric methods for analysis of drug in bulk and its capsule dosage form. The optimum conditions for color development had been established by varying the different parameters involved. The methods were optimized for different conditions like pH and volume of buffer solution for both dyes to obtain maximum sensitivity Both methods involve formation of ion-associated complex with BCG and BTB at pH 3.6±0.02 phosphate buffer, exhibiting wavelength of maximum absorbances at 418 nm for BCG and 413 nm for BTB (Figure 2 and 3 respectively).The calibration curve was plotted across absorbance versus concentration and regression equation is calculated from calibration data. (Figure 4 and 5 respectively). For testing Journal of Pharmaceutical and Biomedical Analysis Letters

Figure 3: Spectra of SUM with BTB 275

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Figure 4: Linearity of Sumatriptan Succinate by BCG

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Figure 5: Linearity of Sumatriptan Succinate by BTB

Table 1: Summary of Optical characteristics and Other Parameters S No Parameters BCG BTB 1 Absorption Maxima (nm) 418 413 2 Beer’s-Lambert’srange (μg/ml) 10-200 10-200 3 Regression equation (y)* Y = 0.004 x – 0.041 Y = 0.004x-0.090 4 Slope (b) 0.004 0.004 5 Intercept (a) -0.041 0.090 6 Correlation coefficient (r2) 0.999 0.999 7 Precision (% RSD)** 1.25 0.38 8 Accuracy (% mean recovery) 100.25 100.12 9 Limit of detection (μg / ml) 7.02 5.25 10 Limit of quantification (μg / ml) 23.40 17.50 11 Assay of tablets (%Purity) 99.182 99.65 *y = a + bx; when x is the concentration in mg/ml and y is absorbance unit. **Average of six determinations.

4. Conclusion The proposed spectrophotometric methods were found to be, simple, sensitive, accurate and precise for determination of SUM in capsule dosage form. The common excipients and other additives are usually present in the capsule dosage forms do not interfere in the analysis of SUM in both the methods, hence it can be conveniently adopted for routine quality control analysis of the drug in pharmaceutical formulations.

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5. Acknowledgement We would like thank MSN laboratories, Hyderabad for providing reference sample of SUM. [6]

6. References [1] Tripathi KD. Essentials of Medical Pharmacology, Jaypee Brothers Medical Publishers Pvt.Ltd, New Delhi, 2004, 176. [2] Rajesh Kumar Nayak et. al.,Method Development and Validation of Sumatriptan in Bulk and Pharmaceutical Dosage Forms by UV Spectrophotometric Method. Int J Pharm & Biological Archives, 2011, 2(4): 1100-1105. [3] Buridi Kalyana Ramu, K. Raghubabu. A Simple Colorimetric Determination of Sumatriptan Succinate From Tablet Dosage Forms Using Journal of Pharmaceutical and Biomedical Analysis Letters

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Cobalt Thio Cyanate. Int J Pharm Tech., 2011, 3(4): 1411-1418 K.N. Prashanth,K. Basavaiah and M.S. Raghu. Permaganometric determination of sumatriptan succinate in puredrug and pharmaceutical formulation.Thai J. Pharm. Sci., 2013, 37: 95-106. Kudige N. Prashanth,Kanakapura Basavaiah, And Madihalli S. Raghu. Utilization of NBromosuccinimide As A BrominatingAgent For The Determination of Sumatriptan Succinate InBulk Drug And Tablets. Int J Ana Chem, 2013, 1-11 M.M. Ayad, H.E. Abdellatef, M.M. Hosny, N. Kabil. Utility of Molybdophosphoric Acid in Qualitative And Quantitative Analysis of Sibutramine Hcl, Sumatriptan Succinate And Lomefloxacine Hcl. Int J Pharm Biomed Res., 2012, 3(2):121-126. B. Kalyana Ramu, K. Raghubabu. Ion Association Method For The Determination of Sumatriptan Succinate from Tablet Dosage Forms Using Tropaeolin Ooo. Int J Pharm Sci., 2011, 3(3): 175178. Buridi Kalyana Ramu,G.Rupakumari, K.Ramarao and K. Raghubabu. Development of New Visible 276

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Spectrophotometric Methods For Quantitative Determination of Sumatriptan Succinate Based On Charge-Transfer Complex Formation. Int J Pharm and Pharm Sci Res., 2011, 1(2): 47-51 [9] ICH, Q2 (R1) Validation of Analytical Procedure: Text and Methodology, International Conference on Harmonization, 2005.

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