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![References
1.Gupta P. C method validation of analytical procedures. pharmatutor. 2015;3(1):32-39.
2. Lopez P, Buffoni E, Pereira F, Vilchez Quero J. Analytical Method Validation. Wide
Spectra of Quality Control. 2011;:1-19.
3. [Internet]. Who.int. 2016 [cited 2 March 2019].
https://www.who.int/medicines/areas/quality_safety/quality_assurance/Guideline_Validation
_AnalyticalMethodValidationQAS16-671.pdf
4. Daksh S. VALIDATION OF ANALYTICAL METHODS – STRATEGIES &
SINGFICANCE. International Journal of Research and Development in Pharmacy and Life
Sciences. 2015;4(3):1489-1497. 2424-01-2020](https://image.slidesharecdn.com/seminarvalidation-200302170627/75/Seminar-on-introduction-to-validation-24-2048.jpg)
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Seminar on introduction to validation
- 1. Analytical method validationas per ICH and USP Presented By –Vasanti G. Patil M. Pharm First Yr.(QAT) 2020 Roll No. 26 Guided By – Dr. Sonali Mahaparale 124-01-2020
- 2. CONTENTS Introduction Objective Types of analytical procedures to be validated Validation parameters as per ICH and USP Conclusion Reference 224-01-2020
- 3. Introduction Validation is thedocumented act of proving that any procedure, process, equipment, material, activity or system actually leads to the expected result. or Analytical method validation is a process of documenting/proving that an analytical method provides analytical data acceptable for the intended use. 324-01-2020
- 4. The mainobjective of analytical validation is to ensure that a selected analytical procedure will give reproducible and reliable results that are adequate for the intended purpose. This is applicable to all the procedure either pharmacopoeial or non pharmacopoeial. 424-01-2020
- 5. Types of analyticalprocedures to be validated The required validation parameters also termed “ analytical performance characteristics”, depends upon the type of analytical method. Pharmaceutical analytical methods are characterized into 5 general types Identification tests Potency assays Limit tests for the control of impurities Impurity tests- quantitative Specific tests 524-01-2020
- 6. Validation parameters asper ICH/USP USP Specificity Linearity or range Accuracy Precision Limit of detection Limit of quantitation Ruggedness Robustness ICH Specificity Linearity Range Accuracy Precision Limit of detection Limit of quantitation Robustness 624-01-2020
- 7. Accuracy “The accuracy ofan analytical procedure is the closeness of agreement between the values that are accepted either as conventional true values or an accepted reference value and the value found”. Determination Assay i. Drug substance ii. Drug product iii. Impurities (quantitation) 724-01-2020
- 8. Recommended data: Assessed by9 determinations over a minimum of 3 concentration levels covering a specified range. Limit Typical accuracy of the recovery of the drug substance is expected to be about 99 – 101%. Typical accuracy of the recovery of the drug product is expected to be about 98 – 102%. 824-01-2020
- 9. Precision “The closeness ofagreement (degree of scatter) between a series of measurements obtained from multiple samplings of the same homogeneous sample”. Precision includes: Repeatability Intermediate Precision Reproducibility 924-01-2020
- 10. Repeatability • Repeatability expressesthe precision under the same operating conditions over a short interval of time. • Repeatability should be assessed using a minimum of 9 determinations covering the specified range. Intermediate precision • Intermediate precision expresses variations within laboratories, such as different days, different analysts, different equipment etc. Reproducibility • Reproducibility expresses the precision between laboratories.1024-01-2020
- 11. Following parameters shouldbe reported a. Standard deviation. b. Relative standard deviation. Concentration µg/ml Absorbance SD and %RSD 8 0.337 0.334 0.341 0.00041 1.223% 12 0.575 0.583 0.596 0.0106 1.158% 20 0.967 0.985 0.978 0.0091 0.993% 0 0.2 0.4 0.6 0.8 1 1.2 8 12 20 Absorbance 1124-01-2020
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- 13. LOD and LOQ The limit of detection (LOD) is usually defined as the lowest quantity or concentration of a component that can be reliably detected with a given analytical method. LOQ are terms used to describe the smallest concentration of an analyte that can be reliably measured by an analytical procedure 1324-01-2020
- 14. Determination of LODand LOQ Limit of detection Method Based on visual examination. Based on standard deviation of response and slope. Signal to noise ratio 2:1 or 3:1 Limit of quantitation Method Based on visual examination. Based on standard deviation of response and slope. Signal to noise ratio 1424-01-2020
- 15. Specificity Specificity is theability to assess unequivocally the analyte in presence of components which may be expected to be present. Determination • Identification tests • Assay and impurity test(s) 1524-01-2020
- 16. Linearity The Abilityof the method to obtain test results that are directly proportional to concentration within a given range. Method: dilution of stock solution/separate weightings Minimum 5 concentrations are used 1624-01-2020
- 17. Range The intervalbetween the upper and lower concentrations of analyte in the sample that have been demonstrate to have a suitable level of precision, accuracy, and linearity. Specific range dependent upon intended application of the procedure. 1724-01-2020
- 18. Range(Continued) Assay: 80to 120% of test concentration. Content uniformity: 70 to 130% of test concentration. Dissolution: 20% to 120% Impurities reporting level: 120% of specification limit (with respect to test concentration of API) 1824-01-2020
- 19. Ruggedness The ruggednessof an analytical method is the degree of reproducibility of test results obtained by the analysis of the same samples under a variety of conditions, such as different laboratories, different analysts, different instruments, different days, etc. Certain may include • Source • Concentration and stability of solution • Heating rate • Column temperature • Humidity 1924-01-2020
- 20. Robustness “The robustness ofan analytical procedure is a measure of its capacity to remain unaffected by small, but deliberate variations in method parameters and provides an indication of its reliability during normal usage”. Determination: The evaluation of robustness should be considered during the development phase and depends on the type of procedure under study. 2024-01-2020
- 21. System suitability Systemsuitability testing is an integral part of many analytical procedures. The tests are based on the concept that the equipment, electronics, analytical operations and samples to be analyzed constitute an integral system that can be evaluated as such. System suitability testing has been recommended by USP in HPLC procedures. 2124-01-2020
- 22. Conclusion When themethod is properly validated consistent, reliable and accurate results are obtained. Analytical method validation is an important analytical tool to ensure the accuracy and specificity of the analytical procedures with a precise agreement. Validation of analytical methods is also required by regulations. Hence it is very important to validate any analytical method that has been developed 2224-01-2020
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- 24. References 1.Gupta P. Cmethod validation of analytical procedures. pharmatutor. 2015;3(1):32-39. 2. Lopez P, Buffoni E, Pereira F, Vilchez Quero J. Analytical Method Validation. Wide Spectra of Quality Control. 2011;:1-19. 3. [Internet]. Who.int. 2016 [cited 2 March 2019]. https://www.who.int/medicines/areas/quality_safety/quality_assurance/Guideline_Validation _AnalyticalMethodValidationQAS16-671.pdf 4. Daksh S. VALIDATION OF ANALYTICAL METHODS – STRATEGIES & SINGFICANCE. International Journal of Research and Development in Pharmacy and Life Sciences. 2015;4(3):1489-1497. 2424-01-2020
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