Spectrophotometric method development and validation for the estimatio

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Sireesha P et al / Int. J. of Allied Med. Sci. and Clin. Research Vol-71 2019 17-20 17 IJAMSCR |Volume 7 | Issue 1 | Jan - Mar - 2019 www.ijamscr.com Research article Medical research Spectrophotometric method development and validation for the estimation of ticagrelor in bulk and its dosage forms P. Sireesha 1 A. Ajitha 2 T. Rama Mohan Reddy 3 1 Dept of Pharmaceutical Analysis and Quality Assurance CMR College of Pharmacy Medchal Hyderabad India-501401. 2 Dept of Pharmaceutical Analysis and Quality Assurance CMR College of Pharmacy Medchal Hyderabad India-501401.. 3 Associate Professor department of Pharmaceutical Chemistry CMR College of Pharmacy Medchal Hyderabad-501401. Corresponding Author: A. Ajitha Email id: ajithaazhakesan27gmail.com ABSTRACT Simple sensitive accurate precise stability indicating UV spectrophotometric method have been developed for quantitative determination of ticagrelor in bulk and its dosage form. The UV spectrum was scanned between 200-400 nm and 254 nm was selected as maximum wavelength for absorption. Beer’s law was obeyed in the concentration range of 2-10µg/ml were found the method was successfully applied to the pharmaceutical dosage forms containing the above mentioned drug without any interference by excipients. Results of the analysis were validated as per ICH guidelines. This method can be used for the routine and quality control analysis of ticagrelor in raw material and pharmaceutical formulations. Keywords: Ticagrelor UV Spectrophotometric method Validation. INTRODUCTION The scope of developing and validating analytical method is to ensure a suitable method for a particular analyte more specific accurate and precise 1 . The main objective for that is to improve the conditions and parameters which should be followed in the development and validation.Ticagrelor is an anticoagulant and anti platelet drug it blocks adenosine diphosphate ADP receptors of sub type P2Y12.Ticagrelor is chemically 1S2S3R5S-3-7-1R2S-2-34- difluorophenylcyclopropylamino-5-propylthio- 3H-123triazolo45-Dpyrimidine-3-yl-5-2- hydroxyethoxycyclopentane-12-diol. Literature review revels that Ticagrelor lower the risk of thrombotic cardiovascular events in patients suffering from coronary syndrome 1 . UV spctrophotometric method is best analytical method for the determination of Ticagrelor 1 .Extensive survey revealed that number of methods has been reported for estimation of Ticagrelor 2 . The aim of the present work is to develop a new simple rapid reproducible inexpensive and efficient linear spectrophotometric method for the estimation of ticagrelorin bulk and its tablet dosage forms. ISSN:2347-6567 International Journal of Allied Medical Sciences and Clinical Research IJAMSCR

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Sireesha P et al / Int. J. of Allied Med. Sci. and Clin. Research Vol-71 2019 17-20 18 Fig 1: Chemical structure of Ticagrelor MATERIALS AND METHODS Ticagrelor dosage form provide AstraZenecapharma India Ltd.Label claim 90mg GR Grade acetonitrile and LR Grade Methanol were procured from SD Fine chem Ltd. Water Whatmann Filter paper. Apparatus Weighing balance UV- Visible Spectrophotometer Spectral and absorbance measurements were made on a UV- Visible spectrophotometer with 10mm Matched pair of quartz cell and spectral band width of ± 2nm. Volumetric flask Pipette Sonicator Hot air oven. UV Method Development Preparation of Ticagrelor standard stock solution Stock solution 10µg/ml of Ticagrelor sample was prepared by transferring 10 mg accurately weighed into a 10 ml volumetric flask and adding 5 ml acetonitrile .The solution was sonicated for 2 min to dissolve Ticagrelor and the solution was then diluted to volume with the same solvent. Further pipette out 1 ml of this solution and dilute up to 10 ml with acetonitrile .100µg/ml. Further pipette out 2.5 ml of this solution and dilute up to 25 ml with acetonitrile. 10µg/ml. Preparation of Calibration curve Calibration curve was constructed in accordance with optimum conditions. Aliquot of standard Ticagrelor solution 100µg/ml was transferred into volumetric flask. At respect concentration 2 µg/ml 4 µg/ml 6µg/ml 8µg/ml and 10µg/ml and the absorbance was measured at 254nm.The solution we scanned in the range of 200-400nm against Acetonitrile as blank. A calibration cure was plotted against Absorbance and concentration. The optical characteristics are summarized in Table no 1. Table no: 1 Calibration curve S.no Concentration µg/ml Absorbancenm 1. 2 0.097 2. 4 0.165 3. 6 0.23 4. 8 0.298 5. 10 0.370

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Sireesha P et al / Int. J. of Allied Med. Sci. and Clin. Research Vol-71 2019 17-20 19 Fig: 2 Determination of λmax of Ticagrelor by UV spectrophotometer Assay of Ticagrelor in Dosage Forms Ten tablets were taken and powered. Weigh a quantity equivalent to 90mg of ticagrelor and transferred into 100ml volumetric flask and dissolve in a small quantity of acetonitrile. The Solution was sonicated and followed by filtration. The first few ml was discarded and the resulting solution is further diluted to produce required concentration. The absorbance was measured at 254nm using Acetonitrile as blank. The maximum absorbance of sample was found to be 0.21 at 254nm. UV- method validation Accuracy Accuracy should be reported as percent recovery by the assay of known added amount of analyte in the sample or as the difference between the mean and the accepted true value together with the confidence intervals. Table no: 2 Accuracy of Ticagrelor Brand name Label claim Amount of drug estimated label claim Standard deviation Ticagrelor 90mg 89.3 99.2 .102 Precision The degree of agreement between an individual test result when the procedure is applied repeatedly to multiple samplings. it is expressed as relative standard deviation. The reproducibility of the proposed method were determined by performing the tablet assay at different intervals of same day intra -day and three different days inter day.the result of intra- day and inter-day was expressed in RSD. Here the study of precision was analysed by measuring the same concentration 6µg/ml in six replicate readings. Table no: 3 Intraday precision Concentrationµg/ml Absorbance 1 Absorbance 2 Absorbance 3 6µg/ml 0.230 0.234 0.232 6µg/ml 0.232 0.234 0.230 6µg/ml 0.234 0.231 0.230 6µg/ml 0.231 0.230 0.233 6µg/ml 0.230 0.234 0.234 6µg/ml 0.234 0.234 0.232 RSD 0.78 0.79 0.69 Average RSD 0.75

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Sireesha P et al / Int. J. of Allied Med. Sci. and Clin. Research Vol-71 2019 17-20 20 Table no: 4 Inter day precision Concentrationµg/ml Absorbance 1 Absorbance 2 Absorbance 3 6µg/ml 0.233 0.234 0.232 6µg/ml 0.230 0.232 0.237 6µg/ml 0.234 0.233 0.234 6µg/ml 0.232 0.234 0.235 6µg/ml 0.234 0.235 0.236 6µg/ml 0.232 0.234 0.234 RSD 0.64 0.76 0.74 Average RSD 0.71 Linearity The linearity of the response of the drug was verified at 2-10µg/ml concentration. The calibration graph was obtained by plotted the absorbance versus the concentration data and was treated by linear regression analysis..... The equation of the calibration curve for Ticagrelor obtained y 0.034x + 0.028 the calibration curve was found to be linear in the above mentioned concentrations. The correlation coefficient r 2 of determination was 0.999. Table for all parameters S.no Parameters Results 1 Absorption maxima nm 254nm 2 Linearity range µg/ml 2-10 3 Standard regression equation y 0.034x + 0.028 4 Correlation coefficient r 2 0.999 5 Accuracy 102 6 Precision 0.75 intraday 0.71 inter day REFERENCES 1. M. A. Ambasana N. P. Kapuriya K. M. Mangantani K. D. Ladva.An improved assay method for the estimation of ticagrelor HCL by RP-HPLC. International journal of pharmaceutical since. 2016. Vol 7. 2. Introduction of ticagrlor by National institute for health and excellence Nice technology appraisal guidance 2011 236 1 3. L. Kalyani A. LakshmanaRao spectrophotometric method development and validation of estimation of ticagrelor in bulk and its dosage form Int. J. of Pharm. 2013 3 634. 4. ICH Harmonised Tripartite Guideline. Q2R1 Validation of Analytical Procedures: Text and Methodology. International Conference on Harmonisation 2005 5. www.google.com 6. www.drugs.com 7. www.fda.gov 8. www.mims.com/India How to cite this article: P. Sireesha A. Ajitha T. Rama Mohan Reddy. Spectrophotometric method development and validation for the estimation of ticagrelor in bulk and its dosage forms. Int J of Allied Med Sci and Clin Res 2019 71: 17-20. Source of Support: Nil. Conflict of Interest: None declared.

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