The objective of this study was to evaluate Fourier transform infrared (FTIR) spectrometry to measure milk ketone bodies to detect hyperketonemic cows and compare this method with milk fat to protein ratio to detect hyperketonemia. Plasma and milk samples were obtained weekly from calving to wk 9 postpartum from 69 high-producing dairy cows. The reference test for hyperketonemia was defined as plasma concentration of β-hydroxybutyrate (BHBA) ≥1,200 μmol/L. The weekly prevalence of hyperketonemia during the first 9 wk of lactation was, on average, 7.1%. Both BHBA and acetone in milk, determined by FTIR, had a higher sensitivity (80%) to detect hyperketonemia compared with milk fat to protein ratio (66%). Specificity was similar for the 3 diagnostic tests (71, 70, and 71%). In conclusion, FTIR predictions of BHBA or acetone in milk can detect cows with hyperketonemia in early lactation with a higher accuracy compared with the use of milk fat to protein ratio. Because of the high proportion of false-positive tests, there are concerns about the practical applicability of FTIR predictions of acetone, BHBA, and fat to protein ratio in milk to detect hyperketonemic cows.