Garlapati, Prasanthi (2012) Method Development and Validation of Sitagliptin and Simvastatin in Tablet Dosage form by RP-HPLC. Masters thesis, C. L. Baid Metha college of Pharmacy, Chennai.
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Abstract
The present study combination dosage form selected for the present study contains Simvastatin and Sitagliptin in solid oral dosage forms, recently this combination has been approved by USFDA ( united states food drug administration) in the year 2011. The aim of work is to develop and validate a simple, precise, accurate and economical RPHPLC method as per ICH guidelines for the estimation of Simvastatin and Sitagliptin in bulk and pharmaceutical dosage forms. PLAN OF WORK: To develop a new RP-HPLC method for the simultaneous estimation of Simvastatin and Sitagliptin. To validate the developed method by determining the validation parameters. CONCLUSION: In the present work, an attempt was made to provide a newer, sensitive, simple, accurate and low cost RP-HPLC method. It is successfully applied for the determination of Sitagliptin and Simvastatin in pharmaceutical preparations without the interferences of other constituent in the formulations. In this method, HPLC conditions were optimized to obtain, an adequate separation of eluted compounds. Initially, various mobile phase compositions were tried, to get good optimum results. Mobile phase and flow rate selection was based on peak parameters (height, tailing, theoretical plates, run time etc). The system with Mixed Phosphate Buffer: acetonitrile (25:75) with 0.8 ml/min flow rate is quite robust. The optimum wavelength for detection was 254nm at which better detector response for the both drugs were obtained. The average retention time for Simvastatin and Sitagliptin were found to be 2.475 and 6.528. In specificity it is found that there is no interference of any placebo and blank peaks with the drugs of the analysis concern. The calibration was linear in concentration range of 80-120 μg/ml for Sitagliptin and 16-24 μg/ml for Simvastatin respectively. The sensitivity for the both drugs has been calculated and the LOD and LOQ of the Sitagliptin was found to be 3.0 μg and 9.95μg and for Simvastatin was found to be 3.14μg and 10.01μg. The low values of % R.S.D. indicate the method is precise and accurate. The mean recoveries were found in the range of 99.67 – 100.27 % for Sitagliptin and 99.42 – 100.54% for Simvastatin respectively.Ruggedness of the proposed methods was determined by analysis of aliquots from homogeneous slot by different analysts, using similar operational and environmental conditions; the % R.S.D. reported was found to be less than 2 %. The proposed method was validated in accordance with ICH parameters and the results of all methods were very close to each other as well as to the label value of commercial pharmaceutical formulation. Therefore, there is no significant difference in the results achieved by the proposed method. Hence it is suggested that the proposed isocratic RP-HPLC methods can be effectively applied for the routine analysis of Simvastatin and Sitagliptin in tablet formulation.
| Item Type: | Thesis (Masters) |
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| Uncontrolled Keywords: | Sitagliptin; Simvastatin; RP-HPLC |
| Subjects: | PHARMACY > Pharmaceutical Analysis |
| Depositing User: | Ravindran C |
| Date Deposited: | 20 Oct 2017 05:27 |
| Last Modified: | 20 Oct 2017 05:27 |
| URI: | http://repository-tnmgrmu.ac.in/id/eprint/3688 |
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