Abstract: We developed a new method for chiral separation of fourteen amino alcohols by nonaqueous capillary electrophoresis (NACE) with the D-(+)-gluconic acid δ-lactone-boric acid complex as chiral selector. In order to achieve good enantioseparation, the effects of D-(+)-gluconic acid δ-lactone and boric acid concentrations, triethylamine concentration, as well as capillary temperature were systematically investigated. The optimized conditions were identified as follows:an uncoated fused silica capillary of 50 μm ID with a total length (Ltot) of 55 cm and an effective length (Leff) of 45 cm; 200 mmol·L^-1 D-(+)-gluconic acid δ-lactone, 80 mmol·L^-1 boric acid, and 57.4 mmol·L^-1 triethylamine in methanol; positive pressure injection at 2.9 psi for 2 s; capillary temperature, 25 ±0.2℃; applied voltage, +15 kV; detection wavelength, 214 nm. Under the optimized conditions, a good chiral resolution was achieved in most of the tested drugs. This method provides a foundation for the development and application of new chiral selectors of polyhydroxy compound-boric acid complexes in chiral drugs analysis by NACE.