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See all Premium member Presentation Transcript SEMINAR ONVALIDATION : SEMINAR ONVALIDATION PREPARED BY: Mr. Mahesh Dhalwade GUIDED BY: Prof. U.S. Bagul SIOP PUNE Slide 2: According to the Food and Drug Administration (FDA), validation is : “establish documented evidence which provides a high degree of assurance that a specific process will consistently produce a product meeting its predetermined specifications and quality attributes.” 1 January 2011 2 Purpose of Validation : Purpose of Validation Method is suitable for its intended purpose to get consistent, reliable and accurate data. Identification of Sources and Quantization of Potential errors Satisfy FDA Requirements Establish Proof that a Method Can be Used for Decision Making 1 January 2011 3 Advantages : Advantages Increased output Reduction in rejections and reworking cost effective Avoidances of capital expenditures Reduced testing in-process and in finished goods Easier maintenance of equipment 1 January 2011 4 When should be validated : When should be validated Changes in established methods New method developed for a particular problem Established method used in different laboratories, different equipment or different staff Out-of-control situations within internal quality assurance Demonstration of equivalence between two methods (e.g. a rapid new test against a standard method) 1 January 2011 5 Validation component : Validation component Man Machine Material Method 1 January 2011 6 Types of validation : Types of validation Analytical method validation Equipment validation Process validation Cleaning validation Raw material validation Finished material validation 1 January 2011 7 Part I Analytical Method Validation : Part I Analytical Method Validation the process of demonstrating that analytical procedures are suitable for their intended use and that they support the identity, strength, quality, purity and potency of the drug substances and drug products 1 January 2011 8 Slide 9: 1 January 2011 9 Specificity/Selectivity : Specificity/Selectivity Ability to assess unequivocally the analyze in the presence of components which may be expected to be present. Selectivity describes the ability of an analytical method to differentiate various substances in a sample. 1 January 2011 10 Slide 11: Selectivity: If an analytical procedure is able to separate and resolve the various component of a mixture and detect analyte qualitatively 2. Restricted qualitative detection of the components of a sample Specificity: If the method determines or measures quantitatively the component of interest in the sample matrix without separation Restricted quantitative measurement of one or more analyte 1 January 2011 11 Linearity : Linearity Ability to elicit test results that are directly or by a well defined mathematical transformations proportional to the concentration of analyte in samples within a given range. Minimum of 5 concentrations are used. R square = 0.999 1 January 2011 12 Range : Range The interval between the upper and lower concentrations of analyte in the sample that have been demonstrate to have a suitable level of precision, accuracy, and linearity. Units % or ppm Highest levels of analyte that have been demonstrated to be determinable for the product 1 January 2011 Slide 14: Range Assay 80 to 120% of test concentration Content uniformity 70 to 130% of test concentration Dissolution Q-20% to 120% Impurities Reporting level – 120% of specification limit (with respect to test concentration of API) Assay & Impurities Reporting level to 120% of assay specification 1 January 2011 14 Accuracy : Accuracy Closeness of the test results obtained by the method to the true value. Assessed using a minimum of 3 concentration levels, each in triplicate (total of 9 determinations) reported as Percent recovery of known amount added or The difference between the mean assay result and the accepted value 1 January 2011 15 Precision : Precision Closeness of agreement between a series of measurements obtained from multiple sampling of the same homogeneous sample under the prescribed conditions”. Repeatability Intermediate Precision Reproducibility 1 January 2011 16 Slide 17: 1 January 2011 17 Slide 18: Detection Limit (DL) Lowest amount of analyte in a sample that can be detected but not necessarily quantities. Estimated by Signal to Noise Ratio of 3:1. Quantization limit Lowest amount of analyte in a sample that can be quantified with suitable accuracy and precision. Estimated by Signal to Noise Ratio of 10:1. 1 January 2011 18 Ruggedness : Ruggedness The effectiveness of an analytical process in face of small environmental/operating conditions, such as: different analyst,equipment,labs etc Effectiveness is measured as changes in the precision or accuracy , expressed as relative SD 1 January 2011 19 Robustness : Robustness Measure of its capacity to remain unaffected by a small but deliberated variation in method parameters and provides an indication of its reliability during normal usage. Variations include: stability of analytical solution, variation of pH in a mobile phase, different column temperature, flow rate. 1 January 2011 20 PART IIEQUIPMENT VALIDATION : PART IIEQUIPMENT VALIDATION It include Design Qualification (DQ) Installation Qualification (IQ) Operational Qualification (OQ) Performance Qualification (PQ) 1 January 2011 21 Design qualification : Design qualification Design qualification is defined as: “Providing documented evidence that the design of the facility and equipments meet the requirements of the user specification and GMP”. 1 January 2011 22 Installation Qualification : Installation Qualification Establishing confidence that process equipment and ancillary systems are capable of consistently operating within established limits and tolerances. 1 January 2011 23 Operational Qualification : Operational Qualification Defined as: “Providing documented verification that the systems and sub-systems perform as intended throughout all anticipated operating ranges”. This step proceeds after the IQ has been performed. define the specification and acceptance criteria 1 January 2011 24 Performance Qualification (PQ) : Performance Qualification (PQ) Third and final phase of validation. Process performance qualification- Establishing confidence that the process is effective and reproducible. Product performance qualification- Establishing confidence through appropriate testing that the finished product produced by a specified process meets all release requirements for functionality and safety. 1 January 2011 25 PART III Process Validation : PART III Process Validation Documented evidence which provides a high degree of assurance that a specific process will consistently produce meeting its predetermined specifications and quality attributes.” Prospective process Validation Retrospective Validation Concurrent Validation Revalidation 1 January 2011 26 Prospective Process Validation: : Prospective Process Validation: It is an validation protocol execution before the process is being commercially used. Generally performed on new drug product. The objective is to demonstrate that the process will work in accordance with process validation protocol. 3 pilot (100 ) batches are prepared. 1 January 2011 27 Retrospective Validation : Retrospective Validation Performed for established products whose manufacturing processes are considered to be stable. In retrospective validation numerical in-process/ end pdt data of historic production batches subjected to statistical analysis. In retrospective validation generally 20-30 batches are analysed. 1 January 2011 28 Concurrent validation : Concurrent validation Used in exceptional cases (low volume products) Not be possible to complete a validation programmed before routine production starts. E.g. when a process is being transferred to a third party contract manufacturer/assemble 1 January 2011 29 Revalidation : Revalidation Performed when there are changes in packaging, formulation, equipment or processes which could impact product effectiveness whenever there are changes in product characteristics 1 January 2011 30 variables of wet granulation : variables of wet granulation 1 January 2011 31 Slide 32: 1 January 2011 32 variables of compression and film-coating : variables of compression and film-coating 1 January 2011 33 variables of tablet packaging : variables of tablet packaging 1 January 2011 34 Slide 35: Guidelines on General Principles of Process Validation, Division of Manufacturing and Product Quality, CDER, FDA, Rockville, Maryland (May 1987). Pharmaceutical Process Validation, Berry, I. R. and Nash, R. A., eds., Marcel Dekker, New York (1993) page no 159-190 Lachman, L., Liberman, H. A. and Kanig, J. L., The Theory and Practice of Industrial Pharmacy, 5th edition, 2007, pg. no. 832-833. www.chem.agilent.com/liabrary/application/59635615.pdf ICH Q2A ICH Q2B http://www.waters.com 1 January 2011 35 Slide 36: 1 January 2011 36 You do not have the permission to view this presentation. In order to view it, please contact the author of the presentation.
validation of analytical method mahesh976 Download Post to : URL : Related Presentations : Share Add to Flag Embed Email Send to Blogs and Networks Add to Channel Uploaded from authorPOINT lite Insert YouTube videos in PowerPont slides with aS Desktop Copy embed code: (To copy code, click on the text box) Embed: URL: Thumbnail: WordPress Embed Customize Embed The presentation is successfully added In Your Favorites. Views: 1313 Category: Education License: Some Rights Reserved Like it (3) Dislike it (0) Added: January 01, 2011 This Presentation is Public Favorites: 6 Presentation Description really nice for all part covered releted to validation Comments Posting comment... By: sujataGule (2 month(s) ago) Very nice presentation sir plz send it to me as it is very important. my mail id is suzi1912@gmail.com thank u sujata Saving..... Post Reply Close Saving..... Edit Comment Close By: hardik_padaliya (8 month(s) ago) sir its nice presentation it very helpful to me plz send me on hardik_padaliya@yahoo.com Saving..... Post Reply Close Saving..... Edit Comment Close By: chandusvcp (8 month(s) ago) superbbbbbbbbbbb Saving..... Post Reply Close Saving..... Edit Comment Close By: ssdevulapalli (10 month(s) ago) Pls send me the ppt to my mail ID: ssdevulapalli@gmail.com Thanks Saving..... Post Reply Close Saving..... Edit Comment Close By: sujanian (12 month(s) ago) plz send this ppt on vineetrana1508@yahoo.com Saving..... Post Reply Close Saving..... Edit Comment Close loading.... See all Premium member Presentation Transcript SEMINAR ONVALIDATION : SEMINAR ONVALIDATION PREPARED BY: Mr. Mahesh Dhalwade GUIDED BY: Prof. U.S. Bagul SIOP PUNE Slide 2: According to the Food and Drug Administration (FDA), validation is : “establish documented evidence which provides a high degree of assurance that a specific process will consistently produce a product meeting its predetermined specifications and quality attributes.” 1 January 2011 2 Purpose of Validation : Purpose of Validation Method is suitable for its intended purpose to get consistent, reliable and accurate data. Identification of Sources and Quantization of Potential errors Satisfy FDA Requirements Establish Proof that a Method Can be Used for Decision Making 1 January 2011 3 Advantages : Advantages Increased output Reduction in rejections and reworking cost effective Avoidances of capital expenditures Reduced testing in-process and in finished goods Easier maintenance of equipment 1 January 2011 4 When should be validated : When should be validated Changes in established methods New method developed for a particular problem Established method used in different laboratories, different equipment or different staff Out-of-control situations within internal quality assurance Demonstration of equivalence between two methods (e.g. a rapid new test against a standard method) 1 January 2011 5 Validation component : Validation component Man Machine Material Method 1 January 2011 6 Types of validation : Types of validation Analytical method validation Equipment validation Process validation Cleaning validation Raw material validation Finished material validation 1 January 2011 7 Part I Analytical Method Validation : Part I Analytical Method Validation the process of demonstrating that analytical procedures are suitable for their intended use and that they support the identity, strength, quality, purity and potency of the drug substances and drug products 1 January 2011 8 Slide 9: 1 January 2011 9 Specificity/Selectivity : Specificity/Selectivity Ability to assess unequivocally the analyze in the presence of components which may be expected to be present. Selectivity describes the ability of an analytical method to differentiate various substances in a sample. 1 January 2011 10 Slide 11: Selectivity: If an analytical procedure is able to separate and resolve the various component of a mixture and detect analyte qualitatively 2. Restricted qualitative detection of the components of a sample Specificity: If the method determines or measures quantitatively the component of interest in the sample matrix without separation Restricted quantitative measurement of one or more analyte 1 January 2011 11 Linearity : Linearity Ability to elicit test results that are directly or by a well defined mathematical transformations proportional to the concentration of analyte in samples within a given range. Minimum of 5 concentrations are used. R square = 0.999 1 January 2011 12 Range : Range The interval between the upper and lower concentrations of analyte in the sample that have been demonstrate to have a suitable level of precision, accuracy, and linearity. Units % or ppm Highest levels of analyte that have been demonstrated to be determinable for the product 1 January 2011 Slide 14: Range Assay 80 to 120% of test concentration Content uniformity 70 to 130% of test concentration Dissolution Q-20% to 120% Impurities Reporting level – 120% of specification limit (with respect to test concentration of API) Assay & Impurities Reporting level to 120% of assay specification 1 January 2011 14 Accuracy : Accuracy Closeness of the test results obtained by the method to the true value. Assessed using a minimum of 3 concentration levels, each in triplicate (total of 9 determinations) reported as Percent recovery of known amount added or The difference between the mean assay result and the accepted value 1 January 2011 15 Precision : Precision Closeness of agreement between a series of measurements obtained from multiple sampling of the same homogeneous sample under the prescribed conditions”. Repeatability Intermediate Precision Reproducibility 1 January 2011 16 Slide 17: 1 January 2011 17 Slide 18: Detection Limit (DL) Lowest amount of analyte in a sample that can be detected but not necessarily quantities. Estimated by Signal to Noise Ratio of 3:1. Quantization limit Lowest amount of analyte in a sample that can be quantified with suitable accuracy and precision. Estimated by Signal to Noise Ratio of 10:1. 1 January 2011 18 Ruggedness : Ruggedness The effectiveness of an analytical process in face of small environmental/operating conditions, such as: different analyst,equipment,labs etc Effectiveness is measured as changes in the precision or accuracy , expressed as relative SD 1 January 2011 19 Robustness : Robustness Measure of its capacity to remain unaffected by a small but deliberated variation in method parameters and provides an indication of its reliability during normal usage. Variations include: stability of analytical solution, variation of pH in a mobile phase, different column temperature, flow rate. 1 January 2011 20 PART IIEQUIPMENT VALIDATION : PART IIEQUIPMENT VALIDATION It include Design Qualification (DQ) Installation Qualification (IQ) Operational Qualification (OQ) Performance Qualification (PQ) 1 January 2011 21 Design qualification : Design qualification Design qualification is defined as: “Providing documented evidence that the design of the facility and equipments meet the requirements of the user specification and GMP”. 1 January 2011 22 Installation Qualification : Installation Qualification Establishing confidence that process equipment and ancillary systems are capable of consistently operating within established limits and tolerances. 1 January 2011 23 Operational Qualification : Operational Qualification Defined as: “Providing documented verification that the systems and sub-systems perform as intended throughout all anticipated operating ranges”. This step proceeds after the IQ has been performed. define the specification and acceptance criteria 1 January 2011 24 Performance Qualification (PQ) : Performance Qualification (PQ) Third and final phase of validation. Process performance qualification- Establishing confidence that the process is effective and reproducible. Product performance qualification- Establishing confidence through appropriate testing that the finished product produced by a specified process meets all release requirements for functionality and safety. 1 January 2011 25 PART III Process Validation : PART III Process Validation Documented evidence which provides a high degree of assurance that a specific process will consistently produce meeting its predetermined specifications and quality attributes.” Prospective process Validation Retrospective Validation Concurrent Validation Revalidation 1 January 2011 26 Prospective Process Validation: : Prospective Process Validation: It is an validation protocol execution before the process is being commercially used. Generally performed on new drug product. The objective is to demonstrate that the process will work in accordance with process validation protocol. 3 pilot (100 ) batches are prepared. 1 January 2011 27 Retrospective Validation : Retrospective Validation Performed for established products whose manufacturing processes are considered to be stable. In retrospective validation numerical in-process/ end pdt data of historic production batches subjected to statistical analysis. In retrospective validation generally 20-30 batches are analysed. 1 January 2011 28 Concurrent validation : Concurrent validation Used in exceptional cases (low volume products) Not be possible to complete a validation programmed before routine production starts. E.g. when a process is being transferred to a third party contract manufacturer/assemble 1 January 2011 29 Revalidation : Revalidation Performed when there are changes in packaging, formulation, equipment or processes which could impact product effectiveness whenever there are changes in product characteristics 1 January 2011 30 variables of wet granulation : variables of wet granulation 1 January 2011 31 Slide 32: 1 January 2011 32 variables of compression and film-coating : variables of compression and film-coating 1 January 2011 33 variables of tablet packaging : variables of tablet packaging 1 January 2011 34 Slide 35: Guidelines on General Principles of Process Validation, Division of Manufacturing and Product Quality, CDER, FDA, Rockville, Maryland (May 1987). Pharmaceutical Process Validation, Berry, I. R. and Nash, R. A., eds., Marcel Dekker, New York (1993) page no 159-190 Lachman, L., Liberman, H. A. and Kanig, J. L., The Theory and Practice of Industrial Pharmacy, 5th edition, 2007, pg. no. 832-833. www.chem.agilent.com/liabrary/application/59635615.pdf ICH Q2A ICH Q2B http://www.waters.com 1 January 2011 35 Slide 36: 1 January 2011 36