With the availability of the µ-PrepCell (a micro preparative cell) the electrochemical synthesis of metabolites and other REDOX species (e.g., intermediates) becomes feasible within a short period of time.
Typical quantities are in the µg range / minute. Collecting the products over 1 hour or more result in sufficient amounts for identification by modern NMR. Huge time savings can be realized compared to syntehsis by wet chemistry or the expensive and often non-specific enzymatic approaches.
Application of a square wave pulse is beneficial for metabolite synthesis. The main advantage of this pulising technique is a stable current over a long period of time and a constant synthesis yiled.The electrode surface is thereby continuously reactivated, reducing adsorption or fouling, meanwhile high sample concentration can be introduced into the cell for efficient synthesis.
A) Overlay of 8 mass spectra acquired over 3.5 hrs, illustrating the excellent stability of synthesis of the 3 Verapamil metabolites: m/z 196, m/z 291 and m/z 441. (B) Applied square wave pulse settings for synthesis of Verapamil metabolites with E1 800 mV and E2 400 mV and durations of appr. 2 and 1 s, respectively.
After collection and purification by HPLC the individual metabolites can be analyzed by NMR and/or MS and used as reference material.
For more information about Electrochemical Synthesis of Metabolites see tab with References above of contact Antec at info@myAntec.com
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