Cyclodextrin-mediated micellar electrokinetic chromatography and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry for theenantiomer separation of racemorphan in human urine

Micellar electrokinetic chromatography (MEKC) was successfully and convenie ntly applied to the chiral separation with the addition of cyclodextrins (C Ds) as chiral selector to the running buffer. Chiral separation depended on the type of CD; in particular, P-CD was effective for the chiral separatio n of racemorphan. We investigated the optimal conditions of type and concen tration of CD as chiral selector for the routine enantiomeric separation of racemorphan with good reproducibility. The effects of other parameters suc h as buffer pH and detection wavelength were also investigated to obtain th e optimum conditions for the enantiomeric separation of racemorphan. Matrix -assisted laser desorption/ionization time-of-flight mass spectrometry was used for confirmation of racemorphan. The optimal conditions for enantiomer ic separation of the racemorphan were as follows: 50 mM berate buffer at pH 9.4 with 50 mM SDS, 10 mM beta-CD and 20% 1-propanol, 57 cmx50 mu m fused- silica capillary column, and UV detection at 192 nm. Based on the developed method, racemorphan in human urine was also separated and determined using solid-phase extraction and MEKC. (C) 1999 Elsevier Science B.V. All rights reserved.