Urinary excretion of hydroxylysine diglycoside (GGH) or monoglycoside (GH) is known to be a reliable indicator of metabolic status of bone collagen. Although some preparation methods of the standard GGH or GH from different species have been reported, this study demonstrated that the preparation of the GGH or GH from the human urine was more suitable for the analyses of these glycosides. GGH and GH were prepared in two ways : one from the normal human urine and the other from the alkaline hydrolyzate of marine sponge. The adequacy for their use as the standard substances was evaluated by proton NMR and HPLC. The glycosides obtained from the human urine were confirmed to be normal forms. As for the glycosides obtained from marine sponge, it was demonstrated that the glycosides were diastereoisomers. The urinary levels of GGH and GH of the inhabitants in Cd-polluted area were compared with the values obtained from non-polluted subjects. The measurements of GGH and GH were performed by using the glycosides prepared from the normal human urine as the standard substanses. As the results, the urinary GGH or GH levels of the subjects in the Cd-polluted area had wider distribution ranges than those of controls, although there was no significant difference between Cd-polluted subjects and controls.