analytical method qualification

[alicee!]

Hi al,
I have a very typical industry system type question..

I wanted to know about analytical method validation and its pre-activities.
Say, for an HPLC analytical method (i'm working wiht proteins) we do a 'prevalidation' or 'a method qualification' type of exercise where multiple runs for the methods similar to what we do for validation are run. The data generated is used for setting acceptance criteria for the method validation.
I want to know if this is a general practice.
Also, since I think many of you forum users are from the industry, I would like to mainly know from you if this 'method qualification' type activities are done as GMP - Quality control type studies OR are they usually done as part of research division?
Hope to find some answers on the usual practices.
Thanks.

[tom jupille]

First of all, the acceptance criteria should (in principle) be set by the requirements of the analysis. If you are setting them based on what you achieve, then thay are not truly acceptance criteria and validation consists of documenting the quality of the results. Unfortunately, in the "real world", the latter is often the case!

Second, I would prefer that any "pre-validation" not bedone under cGMP in order to allow more flexibility in fixing the inevitable problems.

Third, whichever way you go, be sure that you have an SOP in place to document it.

[grzesiek]

if I may add to tom's comment
"First of all, the acceptance criteria should (in principle) be set by the requirements of the analysis." - which are set by the customer

[alicee!]

thanks both of u for the reply!

right.. the method development acceptability (whether the developed method is suitable or not) is based on the requirements of the analysis.

prevalidation (or method qualification - is there a known difference in the meaning and terminology - which is prefered?) acceptance criteria are also based on the requirements of the analysis (or customer requirements).

further prevalidation data is generated. there i was asking if this is needed to be a cGMP study.
I would agree with tom, that it is prefered that any "pre-validation" not bedone under cGMP in order to allow more flexibility in fixing the inevitable problems.
exactly flexibility..!

I'd like to know if this can be a usual practice..
are there requirements that these be cGMP regulated studies, for submission?
of course, validation is a cGMP study. method development and prevalidation are only seen as supportive to validation?

do let me know what u think and know of the requirements on this..

also, are there are any regulatory suggestions/articles/references available that mention where and how regulated these studies are to be done. would be nice if i cud quote some references..

thanks!

[krickos]

Hi

Well from a strict ICH guideline point of view there is no requirement attached to development or prestudies.
But if you start thinking about it a bit, findings from prestudies/development may touch at validation parameters such as Robustness (which columns works and do not etc) and system suitability (critical resolution etc).

As for the documentation part I can only give some variants that I have seen.

Some tend to do a separate in-house development report and then the formal validation report (can both be in house or external/for submissions directly).
Personally and for a pratical point of view as several agencies expects a signed validation protocol before the validation, I prefer to keep the validation report separated from the development report unless the validation is very straight forward.

[alicee!]

Thanks!
Ya.. there aren't any requirements easily stated for the prevalidation studies. Or are there any? But then there are various different practices.

Validation protocol onwards.. GMP documentation/ QA approved.. that is what we follow.

But method development and/or qualification experiments and qualification documentation.. should it all be QA approved as this is a prerequisite for validation..?