Pijarowska–Kruszyna J, et al. – Purpose of this research was to establish efficient, reliable and fast technique for isolation of the d,l–HMPAO, which would provide the ligand with high purity and free from the meso–diastereomer. In context of the findings, a novel synthesis method of d,l–HMPAO, drug substance for technetium–99m exametazime preparation has been established.