Hi all,heres a question to all validation specialists:
I have to perform a fully validated HPLC-Method for the determination of assay of active substance and its impurities in a drug formulation. The column temperature is 17°C. My problem is, that in my lab theres only one HPLC-system with an column compartment which is able to control 17°C (ambient temperature in the lab is now 25°C to 30°C). In order to be able to use all HPLC-systems I have further verified the method with ambient temperature. The higher temperature caused changes in retention time and resolution, but all peaks (impuries and active substance) are well resolved.
So my question is: What do i have to revalidate if i change the column temperature? (only specificity or full validation)

Thanks for all replies!

Might be better and less time consuming to just purchase a few column compartments which can be cooled to the temp. stated in your validated method. They are not that expensive, relative to all the other work needed to redo the method validation and resubmit the results.

I suggest you demonstrate specificity, and repeatability/accuracy with a control sample that you probably used for the initial validation (6 replicate injections). May want to check robustness (change organic or aqueous pH?) to see if it impacts resolution. Linearity need not be evaluated provided the area or height of the peaks are similar to that at 17C.

I would demonstrate and document equivalent results at the two temperatures, and put into your cGMP file. cGMP permits small differences in temperatures, but doesn't specify what classifies as small. My question is: who would intentionally validate a procedure at 17C unless that low temperature was absolutely required? In my lab we have 1050s that can heat, but not cool, and some 1100s which can cool to about 10C less than ambient, so all new procedures are performed at temperatures of at least 30C.

I would check the method development and/or the method validation report as to why the method was validated at 17C.

If you are going to revalidate I would do it temperature controlled at 30C instead of at ambient.

Tahnks for your replies!
to Anonymous3 and Tom M.:
The method was developed and validated from a contract laboratory. The critical peak-pair shows at 17°C the maximum resolution of 3.0, but is also well resolved at 30°C (resolution 1.4). Anonymous3 mentioned a allowed deviation of the temperature according cGMP. The European Pharmacopoeia allows also a deviation from temperature, but only 10% (maximum allowed temperature would be 18.7°C). So this is not really an ease for my coloumn compartments. Is the allowed deviation according cGMP analogue? What did you mean with cGMP-file?