Solid Phase Derivatization Reactions in HPLC Polymeric Reductions for Carbonyl Compounds

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Abstract
Polymeric reducing agents, such as polymeric borohydride resins, can be successfully utilized in both the pre-and post-column modes, online, at ambient temperatures, in real-time, for the selective chemical reduction of a large number of aldehydes. Other classes of carbonyl derivatives, such as ketones, esters, amides, etc., are totally unreactive under these same polymeric reduction conditions. This particular reducing agent is fully compatible with conventional reversed phase HPLC columns and mobile phases, such as methanol/water, ethanol/water, and acetonitrile/water, in varying proportions. The approach to selective detection in HPLC described here utilizes conventional UV-VIS detection following pre-or post-column reductions that occur on-line. Alternative detection methods could just as readily be utilized. Overall reactions are rapid, quantitative, reproducible, and highly selective. In certain cases, it is possible to realize improved detection limits as a result of aldehyde reductions. Difference chromatography or changes in detector responses for unresolved reactant and product can be used to denote reactions that have occurred on the original analyte(s) of interest. Polymeric reduction columns can be slurry packed at fairly low pressures, and they are stable at elevated HPLC back pressures for prolonged periods of time and use. The use of polymeric reagents in HPLC is a totally general approach to improved specificity, selectivity, and detection limits in all types of organic and inorganic analyses.

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