Analytical method validation
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The document discusses the benefits of exercise for mental health. Regular physical activity can help reduce anxiety and depression and improve mood and cognitive function. Exercise causes chemical changes in the brain that may help protect against mental illness and improve symptoms for those who already suffer from conditions like anxiety and depression.
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This document discusses validation of analytical procedures for drug substances and products. It describes key validation characteristics including specificity, accuracy, precision (repeatability and intermediate precision), detection limit, quantitation limit, linearity, range, and robustness. Validation is required for identification tests, assays of active ingredients and selected components, and tests for impurities. The level of validation depends on the objective and type of analytical procedure.
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What is Validation?
Methods validation is the process of demonstrating that analytical procedures are suitable for their intended use-Guidance for Industry
Validation is a process-risk will determine the effort
High Risk:Total validation
Moderate Risk:Testing,Documentation
Low Risk:Testing the change
Validation of Analytical Methods-Key Steps
Preparation
Experimentation
Transfering Method
Documentation
Step 1- Preparation
Develop validation project plan
Define purpose/scope of method (performance criteria)
Define and verify performance of equipment
Qualify/validate materials
Qualify/train operator
Step 2- Experimentation
Perform validation experiments- may have to change either equipment or limits
Develop SOPs for executing the method in routine
Define type and frequency of system suitability tests and/or analytical quality control (AQC) checks
Define change control procedure
Document validation experiments and results
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Designate project owner
Develop procedure on how to use method
Develop system suitability tests (test procedure, frequency, acceptance criteria)
Define transfer tests and acceptance criteria in the routine
Train routine lab analyst in development lab
Repeat 2 critical method validation tests in routine lab
Analyze at least three samples in development and routine lab
Analyst in routine lab should give frequent feedback
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Objective, scope
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Materials
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Transfer to routine protocol
Reference to SOP
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The document discusses analytical method validation. It defines validation as establishing evidence that a process will consistently produce a product meeting predetermined specifications. The objectives are to discuss aspects of validation including principles, approaches, and characteristics. Key steps in validation are establishing accuracy, precision, specificity, linearity, range, limits of detection and quantification, and robustness of analytical procedures used for identification, quantification of impurities and active ingredients.
Method Validation: What Are Its Key Parameters
What is Validation?
Methods validation is the process of demonstrating that analytical procedures are suitable for their intended use-Guidance for Industry
Validation is a process-risk will determine the effort
High Risk:Total validation
Moderate Risk:Testing,Documentation
Low Risk:Testing the change
Accuracy
ICH defines accuracy of an analytical procedure as the closeness of agreement between the conventional true value or an accepted reference value and the value found.
% Accuracy = Experimental- True Value * 100
True Value
Precision
Precision of analytical procedure is defined as closeness of agreement in values between a series of measurements. As per ICH, precision is considered at three different levels:
Repeatability or intra—assay precision: precision data are obtained by repeatedly analyzing, in one lab on one day, aliquots of a homogeneous sample.
Intermediate precision: precision obtained when the assay is performed by multiple analysts, multiple instruments, and multiple days in one lab.
Reproducibility: precision between laboratories.
Specificity
Specificity is the ability of the method to accurately measure the analyte response in the presence of all potential sample components.
It is very important in the analysis of complex mixtures by GC, HPLC, AA, ICP, etc.
Limit of Detection (LOD)
Limit of Detection (LOD) is the lowest amount of analyte in a sample which can be reliably detected but not necessarily accurately or precisely measured.
Signal/Noise = 2 to 3
Limit of Quantitation (LOQ)
Limit of Quantitation (LOQ) is the lowest amount of an analyte that can be quantitatively determined with suitable precision and accuracy.
Signal/Noise = 10 to 20
Linearity and Range
Linearity of an analytical procedure is its ability (within a given range) to obtain test results which are directly proportional to the concentration (amount) of analyte in the sample.
Range: Interval from the upper to the lower concentration (amounts) of analyte in the sample (including these concentrations) for which it has been demonstrated that the analytical procedure has a suitable level of precision, accuracy and linearity
Must cover 80-120% of product claims
Usually evaluated from the same data set as linearity, precision, accuracy
Want to learn more about analytical method validation, FDA requirements and best practices to comply with them? ComplianceOnline webinars and seminars are a great training resource. Check out the following links:
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Assay-Method validation-PPT _slide
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This document summarizes guidelines for analytical method validation from various regulatory agencies. It discusses the purpose of validation to verify method suitability for submissions. Key validation characteristics covered include specificity, linearity, range, accuracy, precision, detection/quantitation limits, robustness, and system suitability testing. It notes that revalidation may be necessary if the analytical method or drug product is changed.
Method validation for drug substances and drug product _remodified_2014
Method validation is the process of proving that an analytical method is acceptable for its intended purposes.
METHOD VALIDATION = ERROR ASSESSMENT
Method validation is 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
Validation: Prior Considerations Suitability of Instrument Status of Qualification and Calibration Suitability of Materials Status of Reference Standards, Reagents, Placebo Lots Suitability of Analyst Status of Training and Qualification Records Suitability of Documentation Written and approved standard test procedure and proper approved protocol with pre-established acceptance criteria
Compendial vs. Non-compendial Methods
Compendial methods-Verification
Regulatory analytical procedure in USP/NF
Non- compendial methods-Validation
Alternative analytical procedure proposed by the applicant for use instead of the regulatory analytical procedure
Chromatographic Methods
Demonstrate Resolution
Impurities/Degradants Available
Spike with impurities/degradants
Show resolution and a lack of interference
Impurities/Degradants Not Available
Stress SamplesFor assay, Stressed and Unstressed Samples should be compared.
Ability of an analytical method to measure the analyte free from interference due to other components.
Selectivity describes the ability of an analytical method to differentiate various substances in a sample
Original term used in USP
Also Preferred by IUPAC and AOAC
Also used to characterize chromatographic columns
Degree of Bias (Used in USP)
The difference in assay results between the two groups
the sample containing added impurities, degradation products, related chemical compounds, placebo ingredients
Selectivity: For impurity test, impurity profiles should be compared.
Temperature (50-60℃)
Humidity (70-80%)
Acid Hydrolysis (0.1 N HCl)
Base Hydrolysis (0.1 N NaOH)
Oxidation (3-30%)
Light (UV/Vis/Fl)
Intent is to create 10 to 30 % Degradation
Change in the analytical procedure, drug substance, drug product, the changes, may necessitate revalidation of the analytical procedures.
“The degree of revalidation depends on the nature of the change.”
“FDA intends to provide guidance in the future on post-approval changes in analytical procedures.”
By Visual Inspection of plot of signals vs. analyte concentration
By Appropriate statistical methods
Linear Regression (y = mx + b)
Correlation Coefficient, y-intercept (b), slope (m)
Acceptance criteria: Linear regression r2 > 0.999
Requires a minimum of 6 concentration levels
Normally derived from Linearity studies.
Established by confirming that the method provides acceptable degree of linearity, accuracy, and precision.
Specific range dependent upon intended application of the procedure.
Validation of Analytical and Bioanalytical methods
Guidelines for Validation of Analytical and Bioanalytical methods as per ICH (Q2R1) and USFDA respectively with an example of Bioanalytical method validation.
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1. The document provides an overview of method validation requirements from various regulatory bodies and guidelines. It discusses key validation parameters such as specificity, linearity, range, accuracy, precision, detection limit, and quantitation limit.
2. Validation is required to demonstrate that analytical methods are suitable for their intended purposes. It identifies potential sources of error and quantifies errors in the method. Validation includes parameters like linearity, range, accuracy, and precision.
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Prepared By :
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Analytical method validation’s superlative characteristic, linearity is comprehensively explained in this slide show. Linearity commonly understood as proportional relationship between two units, in context of method validation, it refers toproportional relationship between test results and concentrations.
A Step-by-Step Guide for Method Validation
What is Validation?
Methods validation is the process of demonstrating that analytical procedures are suitable for their intended use-Guidance for Industry
Validation is a process-risk will determine the effort
High Risk:Total validation
Moderate Risk:Testing,Documentation
Low Risk:Testing the change
Validation of Analytical Methods-Key Steps
Preparation
Experimentation
Transfering Method
Documentation
Step 1- Preparation
Develop validation project plan
Define purpose/scope of method (performance criteria)
Define and verify performance of equipment
Qualify/validate materials
Qualify/train operator
Step 2- Experimentation
Perform validation experiments- may have to change either equipment or limits
Develop SOPs for executing the method in routine
Define type and frequency of system suitability tests and/or analytical quality control (AQC) checks
Define change control procedure
Document validation experiments and results
Step 3- Transferring Methods to Routine Laboratories
Designate project owner
Develop procedure on how to use method
Develop system suitability tests (test procedure, frequency, acceptance criteria)
Define transfer tests and acceptance criteria in the routine
Train routine lab analyst in development lab
Repeat 2 critical method validation tests in routine lab
Analyze at least three samples in development and routine lab
Analyst in routine lab should give frequent feedback
Step 4- Documentation for the FDA
Validation report and supporting documentation:
Objective, scope
Methodology
Materials
Equipment
Validation data
Supporting documentation (chromatograms, spectra)
Transfer to routine protocol
Reference to SOP
Want to learn more about analytical method validation, FDA and ICH requirements and best practices to comply with them? ComplianceOnline webinars and seminars are a great training resource. Check out the following links:
ICH, FDA and USP Requirements for Method Validation
How to Validate Analytical Methods and Procedures
Validation of Analytical Methods and Procedures
Eliminate the Confusion - Analytical Method Qualification and Validation
Lifecycle Approach to Analytical Methods with QbD Elements
Analytical Instrument Qualification and System Validation
Lifecycle Approach to Analytical Methods for Drug Products
For more details:http://www.complianceonline.com/validation-of-analytical-methods-and-procedures-webinar-training-701615-prdw?channel=valppt
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This document provides information on cleaning validation and analytical method validation. It discusses key aspects of cleaning validation including protocols, sampling methods, acceptance criteria, and reports. It emphasizes that cleaning validation is important to prevent contamination between products manufactured using the same equipment. It also covers parameters that are important to validate analytical methods such as selectivity, precision, accuracy, linearity, and calibration curves. The document is a reference for professionals on best practices for cleaning validation and analytical method validation.
Analytical method transfer (module 01)
Analytical method transfer involves qualifying a receiving laboratory to perform an analytical test procedure originally developed in a transferring laboratory. It ensures the receiving laboratory has the knowledge and ability to carry out the procedure as intended. There are different types of method transfers, including comparative testing, co-validation between laboratories, revalidation/partial validation, and waivers. Both the transferring and receiving laboratories have responsibilities in the method transfer process, which typically involves testing replicate samples, evaluating acceptance criteria, and documenting the transfer in a protocol.
The Matrix (1999)
The document provides an analysis of the 1999 film The Matrix. It discusses the directors, writers, main stars and various scenes and themes. It analyzes the conversation between Morpheus and Agent Smith and the battle between humans and machines. It also discusses Neo's powers and his efforts to save Morpheus. Overall, the document conducts semiotic, textual, ideological and industrial analyses of The Matrix relating to its symbols, characters, messages and production.
Analytical methods,cleaning validation
This document discusses analytical method validation and cleaning validation in pharmaceutical manufacturing. It defines validation and outlines key parameters assessed in analytical method validation, including linearity, range, specificity, precision, accuracy, detection and quantitation limits, robustness, and system suitability. It also discusses objectives of cleaning validation, levels of cleaning, validation of cleaning processes and equipment, sampling methods, establishment of limits for residues, and documentation requirements. The overall purpose of validation is to demonstrate that processes can consistently produce products meeting specifications.
Analytical method validation
The document discusses analytical method validation. It defines validation as establishing evidence that a process will consistently produce a product meeting predetermined specifications. The objectives are to discuss aspects of validation including principles, approaches, and characteristics. Key steps in validation are establishing accuracy, precision, specificity, linearity, range, limits of detection and quantification, and robustness of analytical procedures used for identification, quantification of impurities and active ingredients.
Method Validation: What Are Its Key Parameters
What is Validation?
Methods validation is the process of demonstrating that analytical procedures are suitable for their intended use-Guidance for Industry
Validation is a process-risk will determine the effort
High Risk:Total validation
Moderate Risk:Testing,Documentation
Low Risk:Testing the change
Accuracy
ICH defines accuracy of an analytical procedure as the closeness of agreement between the conventional true value or an accepted reference value and the value found.
% Accuracy = Experimental- True Value * 100
True Value
Precision
Precision of analytical procedure is defined as closeness of agreement in values between a series of measurements. As per ICH, precision is considered at three different levels:
Repeatability or intra—assay precision: precision data are obtained by repeatedly analyzing, in one lab on one day, aliquots of a homogeneous sample.
Intermediate precision: precision obtained when the assay is performed by multiple analysts, multiple instruments, and multiple days in one lab.
Reproducibility: precision between laboratories.
Specificity
Specificity is the ability of the method to accurately measure the analyte response in the presence of all potential sample components.
It is very important in the analysis of complex mixtures by GC, HPLC, AA, ICP, etc.
Limit of Detection (LOD)
Limit of Detection (LOD) is the lowest amount of analyte in a sample which can be reliably detected but not necessarily accurately or precisely measured.
Signal/Noise = 2 to 3
Limit of Quantitation (LOQ)
Limit of Quantitation (LOQ) is the lowest amount of an analyte that can be quantitatively determined with suitable precision and accuracy.
Signal/Noise = 10 to 20
Linearity and Range
Linearity of an analytical procedure is its ability (within a given range) to obtain test results which are directly proportional to the concentration (amount) of analyte in the sample.
Range: Interval from the upper to the lower concentration (amounts) of analyte in the sample (including these concentrations) for which it has been demonstrated that the analytical procedure has a suitable level of precision, accuracy and linearity
Must cover 80-120% of product claims
Usually evaluated from the same data set as linearity, precision, accuracy
Want to learn more about analytical method validation, FDA requirements and best practices to comply with them? ComplianceOnline webinars and seminars are a great training resource. Check out the following links:
ICH, FDA and USP Requirements for Method Validation
How to Validate Analytical Methods and Procedures
Validation of Analytical Methods and Procedures
Eliminate the Confusion - Analytical Method Qualification and Validation
Lifecycle Approach to Analytical Methods with QbD Elements
Analytical Instrument Qualification and System Validation
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For details vis
Assay-Method validation-PPT _slide
This document discusses analytical method validation for assay methods. It defines validation as demonstrating a method is suitable for its intended purpose. Validation characteristics include precision, accuracy, specificity, linearity, range, ruggedness and robustness. Considerations before validation include calibrated instruments, standardized reagents, trained analysts, test methods and materials. The document describes methodologies for evaluating these characteristics, such as accuracy studies using spiked samples, forced degradation studies for specificity, linearity studies using calibration curves, and ruggedness studies varying analysts, columns, systems and days. Acceptance criteria are provided for each characteristic.
Method-Validation-HPLC-case-study
This document provides an overview of HPLC methodology and validation requirements. It discusses the key components of an HPLC test procedure including system suitability testing, relative response factors, and the validation parameters of specificity, linearity, accuracy, precision, LOD/LOQ, and robustness. Validation requirements depend on whether the method is compendial or non-compendial, with full validation needed for non-compendial methods. System suitability criteria and validation acceptance limits are outlined for various analytical techniques like assay, impurities testing, and dissolution.
Analytical method validation
The document discusses the benefits of exercise for mental health. Regular physical activity can help reduce anxiety and depression and improve mood and cognitive functioning. Exercise causes chemical changes in the brain that may help protect against mental illness and improve symptoms.
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Quality tools (2), Ola Elgaddar, 30 09 - 2013
I) Management and quality tools include planning tools like Hoshin Planning and Gantt charts, as well as team tools like brainstorming and affinity diagrams.
II) Data collection tools mentioned include indicators and check sheets. Indicators are quantitative measures that can help provide data on quality when analyzed. Check sheets are structured forms for collecting and observing data repeatedly.
III) Data analysis tools include control charts to study process changes over time, histograms to show data distributions, and scatter diagrams to show correlations between paired data. Tools for root cause analysis include flow charts, cause-effect diagrams, and Pareto charts.
Bioanalytical Method Validation
The document discusses the development and validation of an LC-MS/MS bioanalytical method for the determination of a drug in human plasma. It describes the objectives, which are to develop a specific, reliable and cost-effective method. It outlines the key steps in method development including literature search, reference standard preparation, extraction procedure selection, and optimization of separation and detection. The validation parameters that will be evaluated are also summarized, including specificity, accuracy, precision, recovery, matrix effects and stability.
Data Analysis Of An Analytical Method Transfer To
To provide the basis for a PDA task force discussion to arrive at a consensus of best industry practices for data analysis of method transfers. The discussion is also relevant to method validation activities.
Analytical Method & Technology Transfer Ispe Guide
This document provides guidance on effectively transferring analytical methods between laboratories. It recommends a standardized process for transferring technology with minimum documentation. This includes establishing acceptance criteria before transfer, executing training at the receiving unit, and issuing a transfer report confirming the receiving unit's qualification. The guidance outlines experimental designs and acceptance criteria for transferring various analytical methods like assay, content uniformity, impurities testing, and dissolution testing. Acceptance criteria are generally based on statistical analyses showing equivalence between laboratory results.
Analytical method validation
This document summarizes guidelines for analytical method validation from various regulatory agencies. It discusses the purpose of validation to verify method suitability for submissions. Key validation characteristics covered include specificity, linearity, range, accuracy, precision, detection/quantitation limits, robustness, and system suitability testing. It notes that revalidation may be necessary if the analytical method or drug product is changed.
Method validation for drug substances and drug product _remodified_2014
Method validation is the process of proving that an analytical method is acceptable for its intended purposes.
METHOD VALIDATION = ERROR ASSESSMENT
Method validation is 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
Validation: Prior Considerations Suitability of Instrument Status of Qualification and Calibration Suitability of Materials Status of Reference Standards, Reagents, Placebo Lots Suitability of Analyst Status of Training and Qualification Records Suitability of Documentation Written and approved standard test procedure and proper approved protocol with pre-established acceptance criteria
Compendial vs. Non-compendial Methods
Compendial methods-Verification
Regulatory analytical procedure in USP/NF
Non- compendial methods-Validation
Alternative analytical procedure proposed by the applicant for use instead of the regulatory analytical procedure
Chromatographic Methods
Demonstrate Resolution
Impurities/Degradants Available
Spike with impurities/degradants
Show resolution and a lack of interference
Impurities/Degradants Not Available
Stress SamplesFor assay, Stressed and Unstressed Samples should be compared.
Ability of an analytical method to measure the analyte free from interference due to other components.
Selectivity describes the ability of an analytical method to differentiate various substances in a sample
Original term used in USP
Also Preferred by IUPAC and AOAC
Also used to characterize chromatographic columns
Degree of Bias (Used in USP)
The difference in assay results between the two groups
the sample containing added impurities, degradation products, related chemical compounds, placebo ingredients
Selectivity: For impurity test, impurity profiles should be compared.
Temperature (50-60℃)
Humidity (70-80%)
Acid Hydrolysis (0.1 N HCl)
Base Hydrolysis (0.1 N NaOH)
Oxidation (3-30%)
Light (UV/Vis/Fl)
Intent is to create 10 to 30 % Degradation
Change in the analytical procedure, drug substance, drug product, the changes, may necessitate revalidation of the analytical procedures.
“The degree of revalidation depends on the nature of the change.”
“FDA intends to provide guidance in the future on post-approval changes in analytical procedures.”
By Visual Inspection of plot of signals vs. analyte concentration
By Appropriate statistical methods
Linear Regression (y = mx + b)
Correlation Coefficient, y-intercept (b), slope (m)
Acceptance criteria: Linear regression r2 > 0.999
Requires a minimum of 6 concentration levels
Normally derived from Linearity studies.
Established by confirming that the method provides acceptable degree of linearity, accuracy, and precision.
Specific range dependent upon intended application of the procedure.
Validation of Analytical and Bioanalytical methods
Guidelines for Validation of Analytical and Bioanalytical methods as per ICH (Q2R1) and USFDA respectively with an example of Bioanalytical method validation.
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