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We report the first example of conopeptide oxidation performed in a biocompatible ionic liquid, 1-ethyl-3-methylimidazolium acetate ([C(2)mim][OAc]), which enables the efficient formation of both hydrophilic and poorly water-soluble conotoxins compared with conventional methods. Moreover, the method features a high-concentration approach ultimately leading to higher yields at reduced separation effort. (c) 2008 European Peptide Society and John Wiley & Sons, Ltd.