A rapid and simple method for determination of mono- and diglycerides in milk and milk products is described. The emulsifiers were extracted from the samples with organic solvents. Soxhlet extraction and supercritical fluid extraction were compared. To avoid interference of the co-extracted triglycerides with mono- and diglycerides during the GC run, triglycerides were separated by solid phase extraction. Then the emulsifiers were silylated and determined by GC-FID. Optimising GC parameters, the contents of mono- and diglycerides could be determined in the same run within 20 min. Mono- and diglycerides were gathered in two separate groups and quantified with betulin as internal standard. Commercial samples were analysed for the presence of mono- and diglycerides. The recovery rates of monoglycerides were about 98% for skim milk and 99% for dessert. Spiked diglycerides were found with 101% in skim milk and 94% in dessert. The limit of determination was 0.001% for mono- and 0.006% for diglycerides.