Chromatography Forum

Many time during the analysis of tablets, we observe that the column goes bad with in few injections i.e. ~ 50-100 injections, even when the mobile phase has a pH in the range of 3-6. Normally this leads to a bad peak shape of one or more peak and decrease in resolution.

Typical anticipated reasons for these are either a dirty sample preparation qulaity of reagents used. I would like to know if there is any good book available on sample preparation which is specifically adressing this area of chromatography and describing ways to identify the root casue of problem.

I think it's clear that if you have a possibility of excipients depositing on the column it will eventually cause an issue detrimental to your analysis. Are you confident the constituents of your sample will be properly eluted? I wouldn't call it a case of "dirty" but rather appropriate sample preparation - our boss even recently wanted us to analyse a relatively small compound as an impurity of a fully substituted long chain fatty acid derivitised sugar by blindly firing it down a C18.. sometimes it boggles the mind.

Contact me. I can send you a book chapter on SPE. While it does not focus specifically on the removal of excipients, it covers many examples of SPE from blood samples to environmental samples.
(from Handbook of Analytical Separations, Vol. 4, I. Wilson editor)