Sieving and air classification are not efficient enough for the extraction of the high-nutritional-value constituents of wheat. The aim of this article is to validate a simple electrostatic separation method of peeling and gluten, which are two such nutriments contained in finely ground wheat grains. The electrostatic separator is composed of metallic grounded belt conveyer and a rotating roll electrode connected to a high voltage supply. The electrostatic behavior of peeling and gluten powders was characterized using surface potential decay and direct charge measurements. These first set of experiments pointed out the conductive behavior of these powders: in contact with a grounded electrode, they lose their charge in less than 10s. In a second set of experiments, mixtures of 50% peeling and 50% gluten powders were processed by electrostatic separation. Experimental design methodology was used to model the outcome of the separation process as function of two control variables: the high-voltage applied to the roll electrode and the speed of the belt conveyor electrode. In this way, it was possible to determine the optimal operational conditions for the recovery of high-purity peeling and gluten fractions.