Revalidation of a method [August 13, 2004]
Posted: Sun Aug 29, 2004 6:45 pm
By Lime on Friday, August 13, 2004 - 02:48 am:
Hi,
I have an HPLC method which is validated in R&D lab. Method requires 3 um particle sized column. I wanted to use same column but has 5 um particle size.So, do i have to revalidate the method.
Thanks a lot..
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By bert on Friday, August 13, 2004 - 03:05 am:
If you use QC samples in the series, revalidation is not neccesary in my opinion.
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By David Blais on Friday, August 13, 2004 - 04:32 am:
Lime,
Can you find a 3 um column to use? It really would put you at much less risk during an inspection by the FDA (or other such governing body).
Short of that, read through the validation report and see what kind of other columns were tested in the robustness studies. If a similar column with 3 um packing material is not listed as an option, I would say the method should be, at the bare minimum, partially revalidated to show equivalence.
Good luck.
-David
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By Mark on Friday, August 13, 2004 - 11:19 am:
David,
Good comments. Might I add my two cents worth though. The USP allows a change in particle size as long as the system suiability is still met for the method. There should have been some system suitability requirements written into the original method and we usually allow changes that are consistent with USP and meet our suitability requirements.
Regards,
Mark
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By Bert on Monday, August 16, 2004 - 01:29 am:
OK Mark, thats my point. If QC demands for accepting a run or batch are not violated, there is no problem. QC aspects can be accuracy/precision/LOQ of reference samples but also system suitability demands.
Bert
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By Lime on Monday, August 16, 2004 - 01:45 am:
Thank you all.
David,
The truth is i don't have any problem about finding 3um sized column. However, we are using this column for cream analyses.So, its plugging in a short time. That's why i wanted to use 5 um sized. Does FDA meet USP requirements? I mean if i follow USP, is it a problem according to FDA ?
Lime
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By David Blais on Monday, August 16, 2004 - 05:06 am:
Lime,
I also perform cream analyses. If your 3um column is plugging in a short time, perhaps you should look to use a guard column and change it frequently. I assume your samples are filtered prior to injection?
Lime (and maybe also Mark),
While the USP allows for changes in Dp as long as system suitability is still met, I believe your internal documents take priority. Since you led me to believe you are running an in-house method (not a USP method), you should consult with your local SOPs. If you are running a USP method, then USP specifications and regulations take priority. If you have not set something up similar to what Mark has done, you may be a little restricted to the changes you can make without proper documentation and perhaps revalidation. Ultimately the FDA (a separate body from the USP) just wants to see you have followed the methods you have in place and meet the specifications you have in place. Whether that is the USP or your in-house documents is up to you.
Bert,
Perhaps I am not understanding you clearly, but if a batch passes QC requirements and is *not* tested via the exact procedures outlined in the SOPs, I would say there is definitely a problem.
-David
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By bert on Monday, August 16, 2004 - 05:32 am:
David,
In my experience, well designed QC/system suitability can provide in-batch validation data in case of minor changes to an SOP, which unfortunately L can not always be prevented. But maybe it also depends on the analytical environment your working in and also the quality system on your lab (GLP/GMP).
regards Bert
-------------------------------------------------------------------------------------------------------
By David Blais on Monday, August 16, 2004 - 10:26 am:
Bert,
Agreed. The management team here tends to err on the side of caution and would rather spend the time and money to revalidate, instead of waiting for an inspection or a review to let us know something is not completed.
David
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By JM on Tuesday, August 17, 2004 - 02:01 am:
I have two points to add,
1. Normally in R&D method development and validations, scientists try to use different column and come to conclusion. If everything is ok with 5 micron column, why one should prefer 3 micron?? ask your R&D. There must be reason for using 3 micron column.
2. As per USP one can REDUCE the particle size not increase .
Hi,
I have an HPLC method which is validated in R&D lab. Method requires 3 um particle sized column. I wanted to use same column but has 5 um particle size.So, do i have to revalidate the method.
Thanks a lot..
-------------------------------------------------------------------------------------------------------
By bert on Friday, August 13, 2004 - 03:05 am:
If you use QC samples in the series, revalidation is not neccesary in my opinion.
-------------------------------------------------------------------------------------------------------
By David Blais on Friday, August 13, 2004 - 04:32 am:
Lime,
Can you find a 3 um column to use? It really would put you at much less risk during an inspection by the FDA (or other such governing body).
Short of that, read through the validation report and see what kind of other columns were tested in the robustness studies. If a similar column with 3 um packing material is not listed as an option, I would say the method should be, at the bare minimum, partially revalidated to show equivalence.
Good luck.
-David
-------------------------------------------------------------------------------------------------------
By Mark on Friday, August 13, 2004 - 11:19 am:
David,
Good comments. Might I add my two cents worth though. The USP allows a change in particle size as long as the system suiability is still met for the method. There should have been some system suitability requirements written into the original method and we usually allow changes that are consistent with USP and meet our suitability requirements.
Regards,
Mark
-------------------------------------------------------------------------------------------------------
By Bert on Monday, August 16, 2004 - 01:29 am:
OK Mark, thats my point. If QC demands for accepting a run or batch are not violated, there is no problem. QC aspects can be accuracy/precision/LOQ of reference samples but also system suitability demands.
Bert
-------------------------------------------------------------------------------------------------------
By Lime on Monday, August 16, 2004 - 01:45 am:
Thank you all.
David,
The truth is i don't have any problem about finding 3um sized column. However, we are using this column for cream analyses.So, its plugging in a short time. That's why i wanted to use 5 um sized. Does FDA meet USP requirements? I mean if i follow USP, is it a problem according to FDA ?
Lime
-------------------------------------------------------------------------------------------------------
By David Blais on Monday, August 16, 2004 - 05:06 am:
Lime,
I also perform cream analyses. If your 3um column is plugging in a short time, perhaps you should look to use a guard column and change it frequently. I assume your samples are filtered prior to injection?
Lime (and maybe also Mark),
While the USP allows for changes in Dp as long as system suitability is still met, I believe your internal documents take priority. Since you led me to believe you are running an in-house method (not a USP method), you should consult with your local SOPs. If you are running a USP method, then USP specifications and regulations take priority. If you have not set something up similar to what Mark has done, you may be a little restricted to the changes you can make without proper documentation and perhaps revalidation. Ultimately the FDA (a separate body from the USP) just wants to see you have followed the methods you have in place and meet the specifications you have in place. Whether that is the USP or your in-house documents is up to you.
Bert,
Perhaps I am not understanding you clearly, but if a batch passes QC requirements and is *not* tested via the exact procedures outlined in the SOPs, I would say there is definitely a problem.
-David
-------------------------------------------------------------------------------------------------------
By bert on Monday, August 16, 2004 - 05:32 am:
David,
In my experience, well designed QC/system suitability can provide in-batch validation data in case of minor changes to an SOP, which unfortunately L can not always be prevented. But maybe it also depends on the analytical environment your working in and also the quality system on your lab (GLP/GMP).
regards Bert
-------------------------------------------------------------------------------------------------------
By David Blais on Monday, August 16, 2004 - 10:26 am:
Bert,
Agreed. The management team here tends to err on the side of caution and would rather spend the time and money to revalidate, instead of waiting for an inspection or a review to let us know something is not completed.
David
-------------------------------------------------------------------------------------------------------
By JM on Tuesday, August 17, 2004 - 02:01 am:
I have two points to add,
1. Normally in R&D method development and validations, scientists try to use different column and come to conclusion. If everything is ok with 5 micron column, why one should prefer 3 micron?? ask your R&D. There must be reason for using 3 micron column.
2. As per USP one can REDUCE the particle size not increase .