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I'm trying to improve peak shape; graphite column

Posted: Tue Sep 26, 2017 4:33 pm
by MestizoJoe
Hello,

I am trying an assay/impurities method for a steroid. The graphite column shows great selectivity but the peak shape needs improvement. So far I have tried a simple gradient with 0.1%TFA and increasing ACN and got a bunch of shark fin peaks which look like mass overload. Not much was loaded though.

I also tried dilute H2SO4 with ACN gradient and H2SO4 with 0.3% SDS and ACN gradient and got poor tailing. Not shark fins but still bad.

I am trying positively charged surfactant next. Good or bad idea?

thanks!