HPLC of intact sulfite adducts

Chromatography Forum: LC Archives: HPLC of intact sulfite adducts
Top of pagePrevious messageNext messageBottom of pageLink to this message  By Anonymous on Tuesday, September 30, 2003 - 04:40 pm:

One popular technique in pharma manufacturing is campaign-style processes. i.e. reactions are carried out in stages and intermediates stored. This style requires less cleaning of reactors where cleaning is required only between stages. One of the potential intermediates which we are developing an HPLC potency and impurities assay is a sulfite adduct similiar to that of structure 2 in the Organic Process Research and Development 2003, 7, 155-160 article:

http://pubs.acs.org/cgi-bin/sample.cgi/oprdfk/2003/7/i02/pdf/op0202235.pdf

However, at low aqueous concentrations required for HPLC, the SO3- group leaves and oxygen forms a double bond. Thus, the sulfite adduct converts to a ketone similiar to the aldehyde (structure number 1 in the above paper). Does anyone known of an HPLC assay where an intact sulfite adduct has been characterized?

Many thanks


Top of pagePrevious messageNext messageBottom of pageLink to this message  By A.Mouse on Wednesday, October 1, 2003 - 08:28 pm:

Need user i.d. to sign on. Thus I do not know your structure.
What is the organic concentration that you need to do HPLC? Are you doing RP? If you use a c18, maybe a large pore C1 gets you to a much lower organic concentration?
Just some idies...


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