The 31P nuclear magnetic resonance spectra of milk from goats, sheep, a rabbit, a baboon and a human were examined and compared with the spectrum of cows' milk. Most of the peaks observed could be assigned to phosphorus compounds already known to be present in such milks. However, rabbit milk was found to contain unexpectedly large amounts of phosphate esters, and to have only low levels of alkaline phosphatase (EC 126.96.36.199) activity. In addition, an unknown compound was detected in baboon milk and in some samples of sheep and goat colostrum. This compound was not identified, but may be a mixed anhydride such as 1,3 diphosphoglyceric acid. The results show that changes during lactation may be followed by 31P nuclear magnetic resonance and that the technique may be of value in authentification of samples.