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The Transfer of Analytical Procedures
Joachim Ermer, Markus Limberger,
Katarzyna Lis, Hermann Wätzig Institut für Medizinische und Pharmazeutische Chemie
der TU Braunschweig h.waetzig@tu-bs.de
www.pharmchem.tu-bs.de/forschung/waetzig.html
1
APV DPhG
Method transfer
R&D developes validated method
Production Method is used in routine QC
Same results in receiving lab?
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The Transfer of Analytical Procedures
• Regulatory Overview
• Planning
• Acceptance criteria, statistics
• Avoiding pitfalls
• Glossary
3. Planning method transfers 3.1. Responsibilities 3.2. Success factors 3.3. Documentation and knowledge transfer 3.4. Definition of transfer types 3.5. Familiarization and training 3.6. Transfer samples 3.7. Transfer protocol 3.7.1. Acceptance criteria 3.8. Experimental investigations 3.9. Finalization of the method transfer, compilation of transfer report
Comparison of results: absolute values
• e.g. means should not differ by more than X units, or by not more than Y%
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• However, if calculations are performed this way, neither variability nor number of repetitions are considered
⇒ n muss festgelegt werden ⇒ nur bei geringer Variabilität, die man großzügig nach oben abschätzen kann
Bei höherer oder schwer abschätzbarer Streuung: Vergleich der Verteilungen
Comparison of results: Student´s t-distribution
• t-test • equivalence tests
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θ CU CL
0
significant, but practically not relevant difference
practically relevant, but not statistically significant difference
θ CU CL
0
low precision. or
low number of samples
the t-test
θ CU CL high precision, or
high number of samples
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+2% -2% 0
Equivalence test : better properties
+2% -2% 0
θ CU CL low precision, or
low number of samples
θ CU CL high precision, or
high number of samples
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+2% -2% 0
+2% -2% 0
θ CU CL low precision, or
low number of samples
θ CU CL high precision, or
high number of samples
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Comparison of intervals avoids the mentioned paradox!
Equivalence test : better properties
The Transfer of Analytical Procedures
Joachim Ermer, Markus Limberger,
Katarzyna Lis, Hermann Wätzig Institut für Medizinische und Pharmazeutische Chemie
der TU Braunschweig h.waetzig@tu-bs.de
www.pharmchem.tu-bs.de/forschung/waetzig.html
12
APV DPhG
The Transfer of Analytical Procedures
J. Ermer a, 1, M. Limberger b, 1, K. Lisb, H. Wätzig c, *
aSanofi-Aventis Deutschland GmbH, Frankfurt, Germany bPhast GmbH, Homburg/Saar, Germany
cUniversity of Braunschweig, Germany
Journal of Pharmaceutical and Biomedical Analysis 85 (2013) 262–276
h.waetzig@tu-bs.de
13 APV DPhG
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