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NH4OH with PLRP, proteins/peptides

Posted: Sat Feb 13, 2010 8:49 am
by DJ
I'm interested in trying different mobile phase as a way to improve selectivity in a multi-step purification scheme.

Peptide standards look fine when run on PLRP with 0.1% TFA and a linear gradient 5-60% MeCN. However, peak shape dramatically deteriorated when 15 mM NH4OH was used in place of TFA. What would cause this?

Perhaps the equilibration time must be longer?

Loading sample on a column equilibrated with 5% MeCN 15 mM NH4OH

My sample volume is 0.4 mL in 10 mM NH4OAc + 250 mM NaClO4, 5% MeCN.

After loading the 0.4 mL sample on to this 1 mm ID PLRP column at 50 ul/min, how long will it take to re-equilibrate with ammonia before beginning the gradient?

Posted: Sat Feb 13, 2010 4:29 pm
by bisnettrj2
In regard to pH changes and the effect on RP separations:

J Sep Sci. 2007 May;30(7):949-63.

Selectivity in reversed-phase separations: general influence of solvent type and mobile phase pH


In regard to what you're asking:

If your standards looked fine with 0.1% TFA, why did you switch to NH4OH? What pH is your mobile phase now? What column are you running?

One more thing - do you mean 0.4 microliters or 0.4 milliliters injected?