α-Lactosamine hydrochloride, substantially free of β-lactosamine hydrochloride; a method of preparing α-lactosamine hydrochloride monohydrate from an anomeric mixture of lactosamine hydrochloride, including: preparing a solution including the anomeric mixture of lactosamine hydrochloride, water and at least one water-miscible organic solvent at a temperature of 0-100° C., and cooling the solution to cause crystallization of α-lactosamine hydrochloride monohydrate; a method of preparing anhydrous α-lactosamine hydrochloride; and use of α-lactosamine hydrochloride as a food supplement or intermediate in synthesis.