Endohedral metallofullerene Ca@C-60 has been prepared by arc-heating o
f graphite rod containing calcium oxide, CaO, and extracted by pyridin
e under the oxygen-free condition. The laser desorption time-of-flight
(LD-TOF) mass spectrum of the pyridine solution exhibits five main pe
aks due to C-60+, Ca@C-60+ C-70+, Ca@C-70+, and C-74+. It has been fou
nd that Ca@C-60 can be extracted only under the atmosphere of degassed
pyridine owing to its high oxygen-sensitivity.