Objective To develop a method to determine the contents of valoilamine and voglibose in the production of voglibose.Methods With the use of Evaporative Light Scattering Detector(ELSD) ELSD2000(ALLTECH,Ltd.)at 95℃,the gas flow rate is 3.0L/min,a SUPELCOSIL LC-NH2(25 cm×4.6 mm,5 μm)column and acetonitrile-water(0.05mol/L ammonium acetate)(80:20)as mobile phase,the flow rate was 1.0 ml/min.Results The calibration curves of valiolamine showed good linearity in the range of 10.11-808.80μg,the average recoveries was 100.8% (n=6), with RSD of 2.52%; The calibration curves of voglibose showed good linearity in the range of 8.10-648.80μg, the average recoverieswas 99.1% (n=6) ,with RSD of 2. 18%; Their resolution is 3. 0. Conclusion　It was proved that the method with HPLC-ELSD was simple, the results were reliable and accurate, it can be used for the quality control in the production of voglibose.