This article presented the advantages of gas chromatography - tandem triple quadrupole mass spectrometer (GC-MSMS) over gas chromatography-mass spectrometer, formulated a calibration method of GC-MSMS equipped with the source of electron impact (EI), by the reference to JJF1164-2006 “Calibration Specification for Bench Top Gas Chromatography-Mass Spectrometers”, and described in details the calibration process。The result data show that the method can be applied to the calibration of this instrument。