Objective To establish a convenient method to determine the inorganic cyanide in human blood by headspace-gas chromatography/mass spectrometry(HS-GC/MS). Methods 1 m L whole blood was used as the sample to be pretreated, then put into a 10 m L headspace vial where to dilute with 1m L deionized water. After addition of 0.5m L phosphoric acid( ≥ 85%), the vial was sealed immediately and heated at 60℃ for 15 min, being kept ready for analysis by HS-GC/MS. An Agilent~? GS-GASPRO chromatographic column(30m×0.32m...