Chromatography Forum

Hi everyone

I'm in the process of drafting an AMT protocol for an LC/ELSD method and would like some help in setting acceptance criteria. The methods are able to detect the following components with their respective concentrations in brackets.
Hypromellose (label claim = 0.25 %)
Polysorbate 80 (label claim = 0.25 %)
Polyaminopropyl biguanide (label claim = 10 ppm)

The concentration of these components are relatively low and I was wondering if we could treat them as impurties and set acceptance criteria based on this. If we use traditional assay limits i.e. % difference between the sending unit and receiving unit we might not be able to meet this stringent requirements. Could anyone advise on apprioate acceptance criteria to set?

Thanks in advance
Mike

Are these excipients and disintegrant given in your finished product specification?

If yes; i) my question is why?
ii) if it is in specification, unfortunately you should set assay limits during method transfer

If no; why do you transfer?

Good luck

Hi

Unfortunaetly we have specifications for them . The method was developed and validated by an contract lab in India and needs to be transfered into our faciltiy. I was wondering if we could apply impurity acceptance criteria. e.g % difference between the sending unit and receiving unit NMT 10%.

Thanks
Mike

Hi

Unfortunaetly we have specifications for them . The method was developed and validated by an contract lab in India and needs to be transfered into our faciltiy. I was wondering if we could apply impurity acceptance criteria. e.g % difference between the sending unit and receiving unit NMT 10%.

Thanks
Mike

What are the acceptance criteria and results of precision (especially intermediate precision) and accuracy limits at the validation report? Maybe this may help to decide and see what you will face with.

Your levels are quite low and tough to achieve eg:2.0%

Hi

The following criteria was used during the validation:

Method precision:
Repeatability - RSD = NMT 5%
Intermediate precison - RSD = NMT 5%, Overall RSD of all 12 preps = NMT 5%

Accuracy:
% Recovery = 95.0 - 105.0%

Regards
Mike

They use an RSD which is normally high for assay, but for these low levels more meaningful and realistic limits..In that case you may prepare your protocol accordingly..

Thanks prepcolumn. I'll use an overall RSD of NMT 5% and use the low concentration as justification. Thanks for all the help/suggestions.

Mike