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Help with Ramipril Assay by Normal Phase

Posted: Thu Jan 25, 2007 11:30 am
by Wormwood
Hi,

After working on a reverse phase method for ramipril successfully for several months now, I now find myself needing to do the same but by normal phase due to a change in sample matrix.

I've initially tried this on various ratio's of hexane:IPA but found that the peak shape was appalling, ramipril tailing massively.

Therefore I switched to Hexane:THF this gave what I took to be a ramipril peak for sample preparations but gave either a much reduced or no peak for the equivalent standard.

Any pointers on likely conditions etc would be greatly appreciated

Posted: Thu Jan 25, 2007 6:32 pm
by Uwe Neue
I don't know if the slow rearrangement of the ramipril is also happening in normal-phase solvents, but this could be the cause of the ugly peak shape. The simplest way to improve this is to increase the temperature.

Posted: Fri Jan 26, 2007 8:40 am
by Wormwood
I suspect the peak shape is probably more to do with interaction with ramipril on the silica, i.e hydrogen bonding issue, which is why I tried THF.

Thanks for the suggestion though I'll give it a try