Robustness--Acceptance limit

we will change analytical method parameters in validation in Robustness.

Eventhough acceptance criteria we met how much of result(Retention time,area) variation acceptable.

Would you pls anyone explain

regards

seshamraju

As such there is not no variation limit mention in any pharmacopiea, but as per industry norm it would be +/- 5.0% and your area should be NMT 2.0% RSD

Hai Abiparate
First of all Thanks for your good reply

I have to tell you some thing about the problem encountered in my method validation recently in one particular method(inhouse,developed in our lab).

We will inject System suitability solution before starting each parameter to check whether the system is suitable or not.

In Validation Report ,all the system suitability injections(injected in each parameter) have to compile in on sheet ,It should also have the same acceptance criteria i.e %RSD for Area Response and RT.

But in Robustness–Change in Flow Rate,Temperature and Wave length… like that both RT and Area were changing as a result in our compilation sheet for stem suitability injections ,It will out of Acceptance criteria.
If I exclude these injections(injected in Robustness) It would be O.K

Regards

Hai Abiparate
First of all Thanks for your good reply

I have to tell you some thing about the problem encountered in my method validation recently in one particular method(inhouse,developed in our lab).

We will inject System suitability solution before starting each parameter to check whether the system is suitable or not.

In Validation Report ,all the system suitability injections(injected in each parameter) have to compile in on sheet ,It should also have the same acceptance criteria i.e %RSD for Area Response and RT.

But in Robustness–Change in Flow Rate,Temperature and Wave length… like that both RT and Area were changing as a result in our compilation sheet for stem suitability injections ,It will out of Acceptance criteria.
If I exclude these injections(injected in Robustness) It would be O.K

Regards

I think that you have to do the stadistical treatment for each parameters, % recovery, tailing, theorical plates, RSD between areas, resolution. You can’t compare the rt from one run to other, neither the areas, because obviously it will change because of the change you made. I think it´s ok inject the suitability solution for evaluate the resolution. Regards!

Retention time is not a system suitability test per se. Although it is expected to be consistent between tests, it is not a part of acceptance criteria. Retention time is given as an identification guidance for the peak. When you change conditions during robustness (eg.flow rate), obviously retention time will change. But this is not considered as a failure.

for system suitability, we prefer to use capacity factor (k’) or relative retention time, if needed, instead of retention time.

[quote=seshamraju]we will change analytical method parameters in validation in Robustness.

Eventhough acceptance criteria we met how much of result(Retention time,area) variation acceptable.

Would you pls anyone explain

regards

seshamraju[/quote]

Hi,

Here is your answer,

Firsr a fall, Robustness is nothing but the degree of effectiveness of analytical method when a small change is made to a method.
we should not have to prove the robustness.
we should have to report the robustness with respect to the extent of change in the method. Eg: Flow rate.

The specification and limits of robustness study should be similar to the precision study.

No need to consider the changes in area and retention time.
consider only System suitability parameters and Results(Eg:assay, % of Impurity)

It should show the reliability of an analysis with respect to deliberate variations in method parameters.
If measurements are susceptible to variations in analytical conditions, the analytical conditions should be suitably controlled or a precautionary statement should be included in the procedure. One consequence of the evaluation of robustness should be that a series of system suitability parameters (e.g., resolution test) is established to ensure that the validity of the analytical procedure is maintained whenever used.

Best Regards,

Bujji Reddy Kanchi.
Validation analyst.
Quality Dept.
Hetero