New rare earth element (REE) data from all lithologies of the Insizwa lobe, Mount Ayliff Complex, are presented. On the basis of size and type of Eu anomaly, the geochemical subdivision of the complex as previously described is sustained and, additionally, the Top Gabbronorite of the Central Zone is shown to have formed from a magma that was compositionally distinct from other Central Zone magmas. The Basal Zone crystallized from magmas with large negative Eu anomalies probably acquired through crustal contamination. Previously recognized compositional heterogeneity in the contact rocks is also a feature of the REE. Overall, the Insizwa magmas had higher La/Sm ratios and, to a lesser extent, higher Gd/Yb ratios than Karoo basalts and appear to have no representatives in the basalt lava sequence of Lesotho.