Analytical Methods for Cleaning Validation
Im Auftrag der ECA Academy

Analytical Methods for Cleaning Validation  Im Auftrag der ECA Academy

Heidelberg, Germany

Seminar Nr. 17075


Kosten

Non-ECA Members: EUR 1790,--
ECA Members: EUR 1590,--
EU GMP Inspectorates: EUR 895,--
APIC Members (does not include ECA membership): EUR 1690,--

Alle Preise zzgl. MwSt.

Rückfragen unter:
Tel.: 06221 / 84 44 0 E-Mail: info@concept-heidelberg.de

Sprecher

Dr Raphael Bar, BR Consulting, Israel

Walid El Azab, STERIS Cooperation, Belgium

Zielsetzung

This course consists of two parts.

The first part revolves around the development of suitable analytical methods. The characteristics of these methods (HPLC, HPTLC, TOC, conductometry, pH, total protein, visual inspection etc…) will be discussed in the light of their capability of detection and quantitation of residues. In particular, the advantages of the TOC method in accurately detecting and quantifying low levels of non-specic residues (such as detergents, drug excipients and active ingredients) which may not be determined by HPLC, will be highlighted. Prior to this, setting Maximal Carry Over (MAC) limits according to PIC/S, FDA and WHO guides will be presented along with the new EMA approach based on toxicity thresholds. Finally, a pre-requisite requirement for a well-developed method is an efficient recovery and therefore, the first part of the course will highlight the various techniques of sample recovery.

The second part of the course will address a systematic validation of the analytical method for cleaning residues. Performance characteristics of the analytical method will be systematically presented, discussed in parallel to guided calculations of examples with Excel.

Hintergrund

Initiating the manufacturing of a pharmaceutical in shared equipment requires demonstrating that no cross-contamination from previous product takes place.

Optimally, residues from a previously manufactured product or API or residues from the cleaning agent itself should be absent or very low. However, here lies the challenge facing an analytical chemist: the need to develop and validate an analytical method that is sensitive enough to detect and reliably quantify well recovered trace amounts of chemicals and practical enough to rapidly deliver results.

Zielgruppe

The addressees of the event are analytical chemists testing the residues, quality control personnel, quality assurance personnel, regulatory affairs professionals and validation personnel also involved in cleaning validation.

The participants should bring a laptop with Excel.

Programm

Introduction

  • Regulations (FDA, EU, PIC/S, APIC, WHO)
  • Types of analytical methods
  • Preparing a method to a validation process
  • Life cycle approach to analytical methods
  • Roadmap to development of analytical methods for cleaning residues
Cleaning Method Characteristics
  • Cleaning procedures in pharmaceutical processes
  • Types of cleaning residues and their identification
  • Development of method for cleaning residues
  • Analytical methods for cleaning residues (HPLC, HPTLC, TOC, Conductometry, pH, total protein, visual inspection etc…)
  • Testing methods for cleaning agents
  • What should you know about a Cleaning Agent
Sampling Techniques of Cleaning Residues
  • Swab and Wipe Sampling
  • Requirements from Swab
  • Rinse Sampling
  • Solvent Sampling
  • Placebo Sampling
  • Product Sampling
  • Visual examination of cleaned equipment
Calculation of Allowable Carryover (MAC)
  • Common MAC limits (PIC/S, FDA and WHO guides)
  • New approach of EMA guide (NOAEL and PDE)
  • Residues limits on swab and rinse samples and in analytical samples
  • Formulas for calculating MAC
Workshop
  • Exercises in calculations of API or drug product residues
  • Exercises in calculations of cleaning agent residues
Specifity of measurement method
  • Interference with excipient residues, degradation product, and cleaning residue
  • Interference with swab extractables
  • Interferences in analytical samples
  • Quantitative aspect of specificity
Accuracy (incl. exercises with Excel)
  • Swab Recovery Studies on coupons
  • Rinse Recovery Studies on coupons
  • Solvent Sampling from hoses
  • Accuracy of the Measurement Method
Precision of measurement method (incl. exercises with Excel)
  • Method Repeatability
  • Intermediate Precision
  • Combined analysis of Repeatability/Intermediate
  • Precision with One-way ANOVA
Detection and Quantitation Limits of measurement methods (incl. exercises with Excel)
  • By ICH, EP and USP methods: Of TOC method, Of HPLC method
  • Visual detection Limit (VDL)
Linearity of measurement method (incl. exercises with Excel)
  • ICH requirements (Correlation coefficient, residual SS, residuals plot)
  • Considerations (number of data points, of repeats, quality of fit to linearity, etc..)
  • Analysis of plot of measured vs. actual concentrations
  • Correlation between Cleaning Validation and Monitoring: Relative TOC response factor of Target Residue/
  • Reference Standard in TOC method
Range
  • Range on swab and rinse samples
  • Range of analytical samples
Robustness
  • Robustness factors for sampling recovery
  • Robustness factors for measurement method
  • by DOE matrix Solvent Sampling from hoses
Documentation of method validation
  • Writing a protocol
  • Writing a report

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