Saravanakumar, M (2015) Analytical Method Development and Validation of Dexketoprofen Tablets by RP-HPLC. Masters thesis, Arulmigu Kalasalingam College of Pharmacy, Krishnankoil.
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Abstract
INTRODUCTION:Analytical chemistry, like other areas of chemistry and science, has gone through drastic changes and growth. Analytical chemistry may defined as the “Science and art of determining the composition of materials in terms of the elements or compounds contained”. In analytical chemistry it is of prime importance to gain information about the qualitative and quantitative composition of substances and chemical species, that is to find out what a substance is composed of and exactly how much. Analytical method is a specific application of a technique to solve an analytical problem. The use of instrumentation is an exciting and fascinating part of chemical analysis that interacts with all areas of chemistry and with many other areas of pure and applied science. Analytical instrumentation plays an important role in the production and evaluation of new products and in the protection of consumers and the environment. This instrumentation provides the lower detection limits required to assure safe foods, drugs and water. The manufacture of materials, whose composition must be known precisely such as substances used in integrated circuit chips, is monitored by analytical instruments. Instrumental or physicochemical methods are based on the theory of relations between the content and the corresponding physicochemical and physical properties of the chemical system being analyzed. Changes in the system properties are either detected or recorded through the measurement of current, electrode potential, electrical conductivity, optical density, refractive index etc. with suitable and sensitive instruments. In instrumental analysis physical property of substance is measured to determine its chemical composition. Measurements of physical properties of analyte such as conductivity, electrode potential, light absorption or emission, mass to charge ratio, and fluorescence, began to be used for quantitative analysis of variety of inorganic and biochemical analyses. Highly efficient chromatographic and electrophoretic techniques began to replace distillation, extraction, and precipitation for the separation of components of complex mixtures prior to their qualitative or quantitative determination. AIM: To validate the as say method for est imation of Dexketoprofen in Dexketoprofen Tablets by HPLC method, and to demonstrate that the analytical procedure is suitable for its intended purpose.OBJECTIVES: On literature survey it was found that Dexketoprofen was estimated by HPLC and UV Spectrophotometric methods, in combination with other drugs in tablet and bulk dosage form. And also no method was available for such estimation in the pharmacopoeia. In view of the need for a suitable method for routine analysis of Dexketoprofen in formulations, attempts are being made to develop simple, precise and accurate analytical methods for estimation of Dexketoprofen and extend it for their determination in formulations. The utility of the developed methods to determine the content of drug in commercial tablet is also demonstrated. Validation of the method was done in accordance with USP and ICH guidelines for the assay of active ingredients. The methods were validated for parameters like accuracy, linearity, precision, specificity, ruggedness, robustness, and system suitability. This proposed method was suitable for the pharmaceutical analysis in analytical laboratories. This method validation protocol provides a high degree of assurance that a specific process will consistently produce that the DEXKETOPROFEN TABLETS 25 mg meeting its predetermined specification, quality characteristics, and to validate the HPLC method using the working standard, Placebo and drug product. RESULT AND DISCUSSION: The objective of the proposed work was method development for the in estimation of Dexketoprofen in tablets by RP-HPLC and to validate the developed method according to USP and ICH guidelines and applying the same for use in the quality control samples in pharmaceutical industry. As there is no official method for the estimation of Dexketoprofen, so we tried to develop a method by which we can quantify the amount of drug present in the given sample. In RP-HPLC method, the conditions were optimized, to estimation of dexketoprofen. Initially, various mobile phase compositions were tried, to got better elution of drug. Mobile phase and flow rate selection was based on peak parameters (height, tailing, theoretical plates, capacity or symmetry factor), run time and resolution. The system with buffer and Methanol: Water (2:48:50) at gradient flow rate of 1.5ml min was found to be quite robust. The optimum wavelength for detection was 260 nm at which better detector response for the drug was obtained. The average retention times for Dexketoprofen was found to be 4.5 min, respectively. According to United States Pharmacopeia, system suitability tests are an integral part of chromatographic method. They are used to verify the reproducibility of the chromatographic system. To ascertain its effectiveness, system suitability tests were carried out on freshly prepared stock solutions. The calibration was linear in various concentration range with correlation. The low values of RSD indicate that the method was precise and accurate. The mean recoveries were found in the range of 98 – 102 %. System precision is evaluated by injecting 10 injections of standard solution and low value of % RSD shows that system is precise. Precision for method is evaluated by analyzing a sample of homogenous batch six times and the low % RSD value shows the method is precise Method robustness was evaluated by alteration of flow rate (±10%), Mobile phase organic content (±5°C), Wavelength (±2 nm) and it was found robust as % RSD was below 2.0%. Ruggedness of the proposed method was determined by analysis of aliquots from homogeneous slot in different laboratories, by different analysts, different column, different system using similar 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 applied for analysis of the same in marketed formulations. Both sample solution and standard solution are stable at 25°C for24 hrs. as the % difference in the area was found to be less than 2.0%. Finally, it can be concluded that the assay values of formulation were the same as mentioned in the label claim with the RSD of < 1.0%. The proposed method was found to be accurate, precise, reproducible and stable, and can be successfully applied for the routine analysis of the drug in tablet dosage forms. CONCLUSION: This assay method by HPLC is validated for statistical parameter and it is found that the analytical procedure for Dexketoprofen tablets 25 mg meets system suitability requirements and acceptance criteria for Specificity, Linearity, Precision, Accuracy, Robustness, Ruggedness parameters and Solution stability. Solution stability study of the standard and sample preparations are found stable for a minimum of 24 hours. There was no deviation obtained during this validation study. Hence, this In-House analytical method is recommended to carry out the assay analysis from now on for this indistinguishable formulation on Dexketoprofen Tablets 25 mg.
| Item Type: | Thesis (Masters) |
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| Additional Information: | Reg. No.261330352 |
| Uncontrolled Keywords: | Analytical Method ; Dexketoprofen Tablets ; RP-HPLC |
| Subjects: | PHARMACY > Pharmaceutical Analysis |
| Depositing User: | Ravindran C |
| Date Deposited: | 03 Apr 2018 07:24 |
| Last Modified: | 03 Apr 2018 09:08 |
| URI: | http://repository-tnmgrmu.ac.in/id/eprint/6824 |
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