A comparative study of the adsorption and desorption processes of methanol in two kinds of nanochannels (i.e. MCM-41 and SWNTs) is performed by in situ continuous-flow laser-hyperpolarized 129Xe NMR. The high sensitivity and short acquisition time of hyperpolarized 129Xe allow for probing the molecular dynamics in a confined geometry under real working conditions. Hyperpolarized 129Xe NMR spectra indicate that the methanol adsorption behavior in nanochannels is determined by the characters of adsorption sites and that the methanol adsorption rate in the nanochannels of SWNTs is faster than in MCM-41. The experimental data shown in this work also indicate that there is a change in gas phase 129Xe NMR signal intensity during the adsorption and desorption of methanol in SWNTs. This may be because there is a strong depolarization of hyperpolarized 129Xe in SWNTs.