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Posted: Wed Oct 14, 2009 11:02 am
by seamoro
trying= varying pH, temperture and organic compostion.............this was mostly performed on the other columns as well

Posted: Wed Oct 14, 2009 11:07 am
by grzesiek
ok, good, do you see in any of your experiments two peaks instead of one, some sign of resolution?

Posted: Wed Oct 14, 2009 11:59 am
by Uwe Neue
How about SymmetryShield?

Posted: Wed Oct 14, 2009 11:59 am
by seamoro
yes........but the problem is the pencilloic acid has 2 peaks, one broad small peak at approx 8mins and the other at 12mins( narrow peak..good peak shape)......so they kinda stretch out over a 5 minute retention. the sodium benzoate is in and around this retention time...so if you separate it from one peak it usually runs into the other!!

Posted: Wed Oct 14, 2009 12:12 pm
by seamoro
we have no SymmetryShield in house...thanks Uwe for sending those papers on solvent and stationary phase selection

Posted: Wed Oct 14, 2009 12:12 pm
by grzesiek
that's kinda interesting :)

is this the acid?
http://en.wikipedia.org/wiki/Penicillic_acid

is it included in pharmacopoeia as impurity? does the Ph states that there shoul be two peaks?

Anyone knows if existence of two forms is pH dependent?

Posted: Wed Oct 14, 2009 12:31 pm
by seamoro
no...its Penicilloic acid of phenoxymethylpenicillin...and yes is an EP impurity. the reason it has 2 peaks ..i think due to its isomer number 1,2 and 3 penicilloic acid.

Posted: Wed Oct 14, 2009 12:44 pm
by grzesiek
could you post structures of these isomers?

Posted: Wed Oct 14, 2009 1:00 pm
by Peter Apps
What is the injection solvent ?

Peter

Posted: Wed Oct 14, 2009 1:02 pm
by seamoro
Phenoxymethylpenicillin Potassium Imp. E (EP): (4S)-2-[Carboxy[(phenoxyacetyl)amino]methyl]-5,5-dimethylthiazolidine-4-carboxylic Acid (Penicilloic Acids of Phenoxymethylpenicillin)

Hope this helps

Posted: Wed Oct 14, 2009 1:11 pm
by grzesiek
I meant the pictures or link to the pictures :?

Posted: Wed Oct 14, 2009 1:12 pm
by seamoro
injection solvent/Diluent= 6.81g KH2PO4 in 1000ml DH20 with adjusted pH with 0.2m NaOH to pH6.5

Posted: Wed Oct 14, 2009 1:49 pm
by danko
Now, why would the pH of the sample solvent be 6.5 whilst the mobile phase’ pH is intended to be 3.5?
I write “intendedâ€

Posted: Wed Oct 14, 2009 2:11 pm
by seamoro
Sorry...i spent the last 30mins trying to transfer the structure to the post..i couldnt do it. I can give you link
http://www.lgcstandards.com/media/559600807.pdf
you will have to download the catalogue...go to page 312 to see its structure.

About the difference of pHs of moblie phase and diluent...well thats the way they have it in the EP!...i thought it was a bit strange as well!

Posted: Wed Oct 14, 2009 2:13 pm
by seamoro
injection volume 20uL