This work investigates the non-equilibrium hydrogenation of biodiesel in an atmospheric pressure cold plasma reactor. We will present our quantitative measurements of the hydrogen atom number density with femtosecond two-photon-absorption laser-induced fluorescence (fs-TALIF). The spatially and temporally resolved hydrogen atom profiles under direct plasma hydrogenation and plasma catalytic hydrogenation with the Ni/Al2O3 catalyst will be measured and further combined with ex situ gas chromatography mass spectrometry (GC-MS) results for further mechanism development. We have shown that hydrogen and argon plasma can saturate more than 90% of C=C bonds at room temperature and atmospheric pressure. Ultimately, we aim to deepen the mechanistic understanding of the non-equilibrium hydrogenation process, which has transformative impacts on plasma applications in alternative fuels.