Estimation of topiramate by colorimetric method rohit bharti
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The document details the development and validation of a colorimetric method for determining topiramate in bulk and oral dosage forms, following ICH guidelines for accuracy, precision, and linearity. It includes specifics on drug solubility, assay method development, recovery studies, and statistical data supporting the method's reliability. The proposed method is deemed simple, accurate, and suitable for routine quality control analysis.
Estimation of topiramate by colorimetric method rohit bharti
- 1. Preesented by Rohit U. Bharati T.Y. B. Pharm. GUIDE Ms. Vandana T. Gawande M.Pharm. (Q.A.) DATE : 21st March 2012 TIME : 02 : 45 p.m. 1
- 2. Sr. No. Particulars 1 AIM & OBJECTIVES 2 INTRODUCTION 3 SELECTION OF DRUG 4 DRUG PROFILE 5 DEVELOPMENT OF ASSAY METHOD 6 VALIDATION METHODS 7 OBSERVATION 8 CONCLUSION 9 BIBLIOGRAPHY 2
- 3. Part A: To developed analytical (UV) method for determination of TOPIRAMATE in bulk and in oral solid dosage form. Part B: To validate developed method as per ICH guidelines for following parameters: a) Accuracy b) Precision d) Linearity and Range e) Limit of Detection f) Limit of Quantitation g) Robustness 3
- 4. COLORIMETRY It is the science & technology used to quantify & describe physically the Human color perception. 4
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- 9. 1. Drugs which not have strong UV absorbance. 2. Drugs for which Colorimetric methods are not available. 3. Drugs for which methods are available but they are time consuming & complex. Eg. Dicloxacillin, Topiramate etc. 9
- 10. TOPIRAMATE Chemical Name 2, 3, 4, 5-bis-o-(1-methylidene)-betaD-fructopyranose sulfamate Solubility freely soluble in acetone, chloroform and ethanol. water it is 9.8 mg/ml. Its saturated solution has a pH of 6.3. Category Anticonvulsant & Antimigraine Drug 10
- 11. 1. Preparation of std. stock solution. 2. Development of colour. 3. Selection of analytical wavelength. 4. selection of analytical concentration Range. 11
- 12. 10 mg of topiramate + distilled water Ultrasonicated (10 min. ) Vol. adjusted with Distilled water (upto 10ml) concentration 1mg/ml 12
- 13. Dilutions of topiramate in Distilled water + 1ml 10% pyridine solution + 1ml 2% ninhydrin solution 20 mins. Cooling at R.T. violet color spectra taken (λ =568nm) 13
- 14. Spectra Of Colour Complex 14
- 15. 1. LINEARITY 2. ACCURACY 3. PRECISION 4. LIMIT OF DETECTION (L.O.D.) 5. LIMIT OF QUANTIFICATION (L.O.Q.) 6. RANGE 7. ROBUSTNESS 15
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- 17. y = 0.0019x + 0.2184 R² = 0.9963 0.9 0.8 0.7 0.6 0.5 0.4 0.3 0.2 0.1 0 0 50 100 150 200 250 300 350 Abs. abs Linear (abs) Conc. Fig. Calibration Curve for TOPIRAMATE at 568 nm Conc. (μg/ml) Absorption 50 0.2999 100 0.413 150 0.5072 250 0.6988 300 0.7679 Table : Linearity of TOPIRAMATE AT 568 nm 17
- 18. Table: Statistical treatment of Recovery data for TOPIRAMATE Level of recovery Conc. Of drug Amt. added absorbance amt. recovered % recovery 80 0.32 0.4 0.5613 0.321 80.47 80 0.32 0.4 0.5595 0.318 79.50 80 0.32 0.4 0.5599 0.319 79.75 100 0.4 0.4 0.6004 0.404 101.00 100 0.4 0.4 0.5998 0.402 100.50 100 0.4 0.4 0.5988 0.400 100.00 120 0.48 0.4 0.6365 0.480 120.00 120 0.48 0.4 0.6366 0.480 120.00 120 0.48 0.4 0.6370 0.481 120.25 18
- 19. Table: Recovery studies of TOPIRAMATE Parameters Level of recovery Level of recovery Level of recovery 80% 100% 120% Concentration added (μg/ml) 0.32 0.4 0.48 Mean of Absorbance 0.5602 0.5996 0.6367 Mean Conc. Recovered (μg/ml) 0.319 0.402 0.480 Mean % recovery 79.90 100.66 120.15 % RSD 0.4785 0.4975 0.1201 19
- 20. System precision : Table: System precision for TOPIRAMATE Replicate Absorbance of TOPI 1 0.4383 2 0.4256 3 0.4204 4 0.4185 5 0.4130 6 0.4231 Mean 0.42315 SD 0.008576 % RSD 1.99 20
- 21. Conc. (μg/ml) Table: Intra-day variability for TOPIRAMATE Absorbance Mean Std dev % RSD Trial 1 Trial 2 Trial 3 100 0.4886 0.4658 0.4557 0.4767 0.00182 0.3826 150 0.4919 0.4779 0.4740 0.4812 0.00941 1.9550 250 0.5855 0.5782 0.5722 0.5786 0.00666 1.1509 21
- 22. Table: Inter-day variability of TOPIRAMATE Conc. (μg/ml) Absorbance Mean Std dev % RSD Day 1 Day 2 Day 3 100 0.4923 0.4687 0.4476 0.4695 0.00476 0.476 150 0.5019 0.4799 0.4777 0.5547 0.00133 0.275 250 0.5995 0.5812 0.5811 0.5872 0.00105 0.180 22
- 23. Limit of Detection (LOD)- 1.823 μg/ ml 3.3 σ S Limit of Quantification (LOQ)- 5.52 μg/ ml 10 σ S Range- 50 - 300 μg/ ml 23
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- 25. A. Analysis of tablet Conc. Of drug (μg) Absorbance Amt. added μg/ml Amt. found in % 100 0.4254 0.4 98.95 100 0.4320 0.4 102.02 100 0.4251 0.4 98.80 100 0.4292 0.4 100.76 100 0.4329 0.4 102.05 100 0.4331 0.4 102.01 25
- 26. ROBUSTNESS Table: Robustness studies Conc. of drug Wavelength at 568 nm Wavelength at 570 nm 100 μg 0.4383 0.5602 100 μg 0.4256 0.5611 100 μg 0.4204 0.5615 100 μg 0.4185 0.5613 100 μg 0.4130 0.5612 Mean 0.42316 0.56106 Std deviation 0.009588 0.000503 % RSD 2.02 0.089 26
- 27. 1. Colorimetric method was developed and validated as per ICH guidelines for estimation of Topiramate in tablets. 2. Development of color is by reaction of amino group of drug with Ninhydrin reagent in presence of pyridine. 3. The method was found to be simple, accurate, precise and specific. Parameters Result Linearity > 0.99 % Recovery 98 – 102 % % RSD < 2 So, the proposed method can be used for the routine quality control analysis of the bulk drug as well as oral dosage forms. 27
- 28. 1. Davidson, A.G., (2002), Ultraviolet-Visible absorption spectrophotometry, In; Beckett, A.H., Stenlake, J.B., Practical pharmaceutical chemistry, 4 th edi., Part-II, CBS Publishers and Distributors, New Delhi, 278- 82. 2. USP 24/ NF 19,The United states pharmacopoeia 24 and National formulary 19, (2000), the United States Pharmacopoeial Convention, Rockville, 1767-69. 3. National Organization for Drug Control and Research, 6 Abou Hazem Street, Pyramids Ave, P.O.Box 29 Giza, `Egypt. (NODCAR) Nahla Nour El-Din Ahmed Salama* et al /International Journal Of Pharmacy. 4. Sanket S.D.1*, Madhuri V. G.1, Shilpa V.1, Mahesh M.D.2, Vikas V.G. International Journal of Pharmaceutical Sciences and Nanotechnology, Volume 2 Issue 4 January – March 2010 5. Davidson,A.G.(2002),Ultraviolet-Visible-absorption spectrophotometry, In; Beckett, A.H., Stenlake, J.B., Practical pharmaceutical chemistry, 4 th edi., Part-II, CBS Publishers and Distributors, New Delhi, 275- 78 28
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