Test Procedure Pre-validation protocol report?

[Consumer Products Guy]

OK, the pointy-haired QA supervisor now wants test procedure pre-validation protocol reports for test method validation in addition to test method validation reports after the project has been completed. Do your companies do this? I can't see anything in the CFR regulations which details needing a pre-validation protocol report. I don't want to set any precedents we don't really need.

[DR]

Just include a summary of decisions in the method validation report (you could call it "development notes" and justify some of the more important choices made by including a few bad/improved chromatograms).

If you've ever asked someone who wrote a method why they chose a particular column and the response was "It was what was left on the system.", you know why the PHB wants this information.

[Yorkie31]

This really does seem like a lot of additional un-required work. It certainly isn't a regulatory requirement that I know about! Oh how I love those Pointy Haired QA types!

DR may have a point in simply putting a quick development one pager together. But no more. Working in the contract industry, this does tend to be the realm of the client wanting to know what their money has been spent on.

As far as QA go, they are strictly there to make sure you are compliant. With regards to development, they have no requirement to know why you made certain decisions with regards to analytical method. If I can stick my neck out here, Analytical Development really isn't a regulated area... it can't be!

If you have written a method, that the validation shows to fulfil its purpose in a compliant manner, that should be all QA need to know!

[Bruce Hamilton]

As far as QA go, they are strictly there to make sure you are compliant. With regards to development, they have no requirement to know why you made certain decisions with regards to analytical method. If I can stick my neck out here, Analytical Development really isn't a regulated area... it can't be!

If you have written a method, that the validation shows to fulfil its purpose in a compliant manner, that should be all QA need to know!

Working as an QC analyst for a contract API manufacturer, I found that every client audit involved inspection of the documentation on method development, starting at the method design stage.

"Why did you choose HPLC technique, that column, solvent, detection method?", and an analyst's workbook or worksheet should have that information in it. Customers tend to get upset if huge amounts of time and effort are invested in validation of a method that has an inherent fault.

A prevalidation report should identify that the the method has been assessed, and is likely to be fit for purpose, and detail what is planned during the validation. Depending on the organisation, you may even have to obtain QA signoff before starting any validation.

Assessment can be as simple as have run all the previous R&D samples to the client's and analyst's satisfaction, or a modification of an accepted published method.

Bruce Hamilton

[bgiles]

We have written development reports indicating the history of the development prior to the validation protocol. Some of the work from development if ran using the final conditions was refrenced in the validation report and not repeated ie solution stability, forced deg, robusteness

the dude

[gbalock]

CG,
We will do a development history and include things done under development like robustness and extration experiments that aren't covered under validation.

Typically we do a pre-validation, but don't write a report on that. It's just to prove that the method is validatable.

I know running the tests is easy, documenting it is hard.

[rc_12321]

It is generally required to maintain a development report when one choose to develop his own method even though compendial method is available.The report basically explains how the in-house method is superior to the one given in a pharmacopeia.

Development ,in fact, includes some validation work too .We generally carry out partial validation during method development stage.These include parameters like stability and filter validation apart from general requirements like placebo and impurity interference .There are some cases where the auditers have asked for method development reports.

[Consumer Products Guy]

Thnaks for the inputs. In THIS case it IS a USP procedure so "of course" this is the first time QA has ever stuck its face into our business. Maybe it's because since they declared themselves "owners" of the test method transfer business 14 months ago, they are 0-3 in getting stuff done correctly. (1) They now demand nine separate samples to be sent because they didn't trust others to assay correctly in triplicate (but they tell them three samples at 80, 100, and 120% of target); unfortunately, that product wasn't very homogeneous, so presampling shot themselves in the foot. (2) QA didn't realize that a product to be produced elsewhere with a new fragrance needed verification to document that the new fragrance didn't interfere with the assay; QA passed a contract lab on transfer samples (sending out trade secret technology by mistake), then at production start-up all results were OOS, so I had the guy go to the contract lab to read me the part number on the HPLC column, and it was NOT the correct column, so we had to do all the assays. (3) for a titration assay taken directly from USP QA had product development make samples at 80, 100, and 120% of target; of course, they didn't have enough jars made to provide 9 jars to all locations, so now potentially-adulterated jars must be re-used at other locations (good thing QA had a meeting to decide how much product needed to be produced). Our validation did prove that the analysts knew how to pipet, good use of resources. For (3), the QA Director and QA Manager didn't even know one of their people had written a QA sOP taking over the whole process (without our input, of course, even though the Appendix included the form I'd been using for a decade). Help, bring on that retirement, it gets nuttier every day. Did I mention that QA has 2.5 times the staff of Analytical Chemistry to "manage" this?

[JM]

CP Guy,
I can relate to what you have been through. The USP or any official method does not require any "method developmet report".

The method transfer is best done by the scientist , who has developed it or validated it. QA should be kept out of it .

To me most of the QA people are " Analytical rejects" avoid them.

JM