A capillary two-dimensional liquid chromatography method coupled with ion trap mass spectrometry has been used for separation and identification of neuropeptides in rat rhinencephalon. Animals of three different age groups were exposed to slow and quick CO2 influx. The neuropeptides were extracted by solid phase extraction and the purified extracts were analysed by 2-D HPLC. The compounds were fractionated (strong cation exchange column), trapped and separated, and MS/MS fragment mass spectra were used for identification. About thirty peptide compounds were identified. A significant difference between concentration levels of "stressed" (quick CO2 influx) and "non-stressed" (slow CO2 influx) rats was found for 25 of the identified peptides.