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Although the only conjugate of pregnanediol (5β pregnane-3,20-diol) in urine is the glucosiduronate (Crepy, Judas, Rulleau-Meslin & Jayle, 1962) when a foetus is perfused with progesterone some pregnanediol sulphate is formed (Bird, Solomon, Wiqvist & Diczfalusy, 1965). There is thus a possibility that pregnanediol sulphate is largely a foetal product and that its measurement may give some indication of foetal well-being. The identification of pregnanediol sulphate in liquor amnii (Solomon & YoungLai, 1969) and the development of a method for the measurement of all the pregnanediol conjugates in amniotic fluid (Klopper, Wilson & Shearman, 1969) has given rise to the opportunity of examining this possibility. In order to do so it was necessary to find out whether the solvolysis technique of Burstein & Lieberman (1958) for ketosteroid sulphates could be adapted to the separation of pregnanediol sulphate and pregnanediol glucosiduronate. We report here the results of such an investigation and