Validation of Analytical Procedures in Pharmaceutical Analysis and Quality Control (2 days)

  Content Day 1
09.00 - 09.30 Regulatory Requirements and Guidelines, Lifecycle Concept
  • cGMPs
  • ICHQ2/Q14
  • USP <1225>, <1220>
09.30 - 10.15 Validation Characteristics: Precision, Accuracy, and Range
  • Error types (random and systematic), (normal) distribution of data 
  • Precision levels, comparison and recovery for accuracy, establishment of range
10.15 - 10.45 Break
10.45 - 11.30 Workshop:  Variability
  • Dispersion of standard deviations and single results & consequences 
11.30 - 12.15 Validation Characteristics: Specificity, Linearity, Detection and Quantitation Limit
  • Direct and indirect demonstration of specificity
  • Parameters of separation, peak purity, response function, calibration
  • General and intermediate QL, determination of QL from linearity, precision, and signal-to-noise ratio
12.15 - 13.30 Break
13.30 - 16.00 Workshop: Design of Validation Studies and Acceptance Criteria for Example Methods
  • Design of validation studies for example methods with respect to the relevant validation characteristics
  • Appropriate experimental approaches, number of series/runs and determinations
  • Selection of suitable calculations and statistical tests, establishment of acceptance criteria
16.00 - 16.30 Break
16.30 - 17.00 Utilisation of Data from Method Development
  • Revision of ICH Q2, prerequisites, documentation
17.00 - 17.45 Maintenance of the Validated Status - Ongoing Performance Verification
  • Lifecycle Stage 3, assurance of appropriate performance after changes
  • Monitoring of performance parameters, continuous improvements
17.45 Final discussion
  Content Day 2
09.00 - 10.30 Workshop: Evaluation of Validation Results for Example Methods
  • The participants are provided with results based on the protocols they have developed in the workshop
10.30 - 11.00 Break
11.00 - 11.30 Workshop: Discussion Precision for Example Methods
  • Presentation of the evaluation
11.30 - 12.00 Requirement-based Acceptance Criteria for Precision
  • Acceptable precision 
  • Empirical and requirement-based, derivation from specification limits for drug substance and drug products
12.00 - 12.30 Determination and Optimisation of Precision
  • Calculation of precision levels by analysis of variances
  • Optimisation of precision of the reportable value by averaging
  • Impact of variance contributions
12.30 - 13.30 Break
13.30 - 14.00 Workshop: Discussion Accuracy for Example Methods
  • Presentation of the evaluation
14.00 - 14.40 Acceptance Criteria for Accuracy
  • Comparison and recovery
  • Appropriate use of statistical tests
  • Impact of variability
14.40 - 15.10 Workshop: Discussion Linearity (Calibration Models) for Example Methods
  • Presentation of the evaluation
15.10 - 15.30 Break
15.30 - 16.00 Requirements to Calibration Models
  • Single-point and multiple-point calibration
  • Statistical linearity tests, regression and concentration range
  • Weighted and unweighted linear regression
  • Suitable and not suitable parameters 
16.00 - 16.30 Workshop: Discussion Detection and Quantitation Limit for Example Methods
  • Presentation of the evaluation
16.30 - 17.15 Detection and Quantitation Limit
  • Distribution of blank and analyte
  • Requirements to a suitable concentration range for linearity-based approaches
  • Potential issues for QL from precision and signal-to-noise
17.15 Final Discussion

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