The primary structure of hypertrehalosaemic factor II, isolated from the corpus cardiacum of the Indian Stick Insect Carausius morosus, has been assigned as Glu-Leu-Thr-Phe-Thr-Pro-Asn-Trp-Gly-Thr-NH2 from its fast atom bombardment (FAB) mass spectrum and metastable scans of its FAB spectrum. The structure assigned shows close homology to other insect neuropeptides. A synthetic sample of this peptide gave the same FAB spectra, reversed-phase high-performance liquid chromatographic behavior, and biological behavior as the natural material. Mass spectrometric fragmentation of the synthetic peptide was examined by B/E linked scan and MIKES techniques in a two-sector mass spectrometer and by the MS/MS technique in a four-sector (tandem) spectrometer.