Elucidation of degradant structures
Posted: Thu Jul 07, 2005 7:35 am
Hello,
I am working on study of degradation products of donepezil hydrochloride.
I have done LC-MS-MS study of donepezil HCl under different stress conditions as per ICH guidelines. The study has been carried out in Q1 mode to obtain Total Ion chromatogram (TIC) in which i got molecualr wts of respective degradant.
only with this data can i propose the structures for degradants?
or any other data is required to do so like IR and NMR?
I have also tried to separate the degradants by micropreparative technique in which i am able to separate two degradation products successfully in degraded sample of donepezil in 6% hydrogen peroxide.
I have MS spectra of both.....it shows the same molecular wt as seen in LC-MS-MS spectrum of same sample.....
so can i confirm structures for those identified degradants?
It was not possible to do NMR and IR due to very limited qty of isolated degardants......and also we didnt have preparative HPLC to get more amts of degardants.
with regards,
Paresh Chothe
M. Pharm Student
I am working on study of degradation products of donepezil hydrochloride.
I have done LC-MS-MS study of donepezil HCl under different stress conditions as per ICH guidelines. The study has been carried out in Q1 mode to obtain Total Ion chromatogram (TIC) in which i got molecualr wts of respective degradant.
only with this data can i propose the structures for degradants?
or any other data is required to do so like IR and NMR?
I have also tried to separate the degradants by micropreparative technique in which i am able to separate two degradation products successfully in degraded sample of donepezil in 6% hydrogen peroxide.
I have MS spectra of both.....it shows the same molecular wt as seen in LC-MS-MS spectrum of same sample.....
so can i confirm structures for those identified degradants?
It was not possible to do NMR and IR due to very limited qty of isolated degardants......and also we didnt have preparative HPLC to get more amts of degardants.
with regards,
Paresh Chothe
M. Pharm Student