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The following message was posted to: PharmPK
Can anyone help with information on European Regulatory requirements for
liquid chromatographic calibration curves.
We have a method that has been subject to extensive validation.
During which
we were able to demonstrate a linear standard curve that passes through
zero. From the FDA Guidance on Bioanalytical Method Development
document, it
is clear that when samples are assayed a full standard curve should be
included in the run.
I assume that it is not possible for FDA submissions to use multiple
replicates (8 per run) of a single concentration and create a single
point
calibration curve that passes through zero - is this correct?
Also, are the requirements of the European Regulators the same as the
FDA in
relation to standard curve requirements, or would they accept a
single point
calibration approach?
Any help would be useful and we are trying to finalise our assay plans.
Andrew
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Hello Andrew,
I've been involved with bioanalytical for 12 years in North America
and thus applying the FDA guidelines.
I've been involved for the last two years with bioanalytical in
Europe and contacted the EMEA and ask them if they had bioanalytical
guidelines.
The reply I got from three different contact was that they need to
know the drug structure in order to provide guidance for the
bioanalytical validation requirements.
I replied if they could provide a similar bioanalytical guidelines as
the FDA but unfortunately did not obtain any feedback from any of
them yet (it's been more than 9 months now).
Until I obtain feedback from the EMEA, I will continue to follow the
FDA bioanalytical method validation guidelines.
Did anyone had a similar experience with either the EMEA or other
European regulatory agencies?
Best regards,
Sylvain
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The following message was posted to: PharmPK
Dear Andrew,
calibration requirements are the same for the US and the EU.
A single point calibrator would not be accepted...
Have a look at this two papers:
SHAH, V.P., MIDHA, K.K., DIGHE, S., McGILVERAY, I.J., SKELLY, J.P.,
YACOBI, A., LAYLOFF, T., VISWANATHAN, C.T., COOK, C.E, MCDOWALL,
R.D., PITTMAN, K.A. and S. SPECTOR;
Analytical methods validation: Bioavailability, bioequivalence and
pharmacokinetic studies
Int. J. Pharm. 82, 1-7 (1992)
SHAH, V.P., MIDHA, K.K., FINDLAY, J.W.A., HILL, H.M., HULSE, J.D.,
McGILVERAY, I.J., MCKAY, G., MILLER, K.J., PATNAIK, R.N., POWELL,
M.L., TIONELLI, A., VISWANATHAN, C.T. and A. YACOBI;
Bioanalytical Method Validation-A Revisit with a Decade of Progress
Pharmaceutical Research 17(12), 1551-1557 (2000)
Best regards,
Helmut
--
Helmut Schuetz
BEBAC
Consultancy Services for Bioequivalence and Bioavailability Studies
Neubaugasse 36/11
1070 Vienna/Austria
tel/fax +43 1 2311746
Web http://BEBAC.at
BE/BA Forum http://forum.bebac.at
http://www.goldmark.org/netrants/no-word/attach.html
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Most often the structure should not influence the validation in any
real way, large molecules can be analyzed with instrumental or
ligand based assays as can small molecules, The only real
exceptions would be for mixtures of different polymers- like
heparin. These may use only PD-prolongation in clotting time as the
endpoint, But the actual components of the validation should be the
same- accuracy, precision, stability etc.
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The following message was posted to: PharmPK
For plasma analysis (BA/BE studies), we use the FDA guidance.
EMEA guidance is provided in the document:
Volume 8, Notice to applicants and Note for guidance Veterinary
medicinal products, Establishment of maximum residue limits (MRLs) for
residues of veterinary medicinal products in foodstuffs of animal origin
We refer to this guidance for validation of residue analysis in edible
tissues.
Regards Bert
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Really we do not have in EU guidelines so detailed as those of FDA.
However, for the analysis of veterinary drugs, we refer to the
following documents:
Direttive 2002/657/CE. Official Journal n. L 221 of 17/8/2002 page
0008 -0036 (for tissues)
The Rules Governing Medicinal Products in the European Union Volume 8
Notice to applicants and guideline. Veterinary Medicinal Products.
Establishement of maximum residue limits (MRLs) for residues of
veterinary medicinal products in foodstuffs of animal origin. October
2005
CVMP/VICH/590/98-FINAL VICH Topic GL1 (Validation: Definition)
Guideline on validation of analytical procedures: definition and
terminology. 10 December 1998
CVMP/VICH/591/98-FINAL VICH Topic GL2 (Validation: Methodology)
Guideline on validation of analytical procedures: methodology. 10
December 1998
Paola Anfossi
Dipartimento di Sanita Pubblica Veterinaria e Patologia Animale
Servizio di Prova di Farmacologia e Tossicologia
Via Tolara di Sopra 50
40064 Ozzano Emilia (BO)
tel. fax +39.051.2097513
e-mail:paola.anfossi.aaa.unibo.it
sito web: http://www.dspvpa.unibo.it/DSPVPA/default.htm
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Copyright 1995-2010 David W. A. Bourne (david@boomer.org)