A new HPLC technique for the separation of methocarbamol enantiomers.

We have developed a stereoselective high-performance liquid chromatography technique for analytical separation of methocarbamol enantiomers. Precolumn derivatization was performed at room temperature using (-)-menthylchloroformate as a chiral reagent in the presence of pyridine as catalyst. The resulting diastereomers were separated on two Resolve C18 columns connected in series. The mobile phase was phosphate buffer (pH 7.5)-acetonitrile (50: 50, v/v) at a flow rate of 1 mL min(-1). UV detection was set at 274 nm. The optimum amount of reagent and the maximum peak intensity of the diastereomers were determined. The resolution of the diastereomers was satisfactory (alpha = 1.04) under the conditions used.