Thomas Gudinas, 51, was scheduled to die by lethal injection at 6:00 pm (2200 GMT) at the Florida State Prison in Raiford.
Gudinas was sentenced to death in 1995 for the murder of Michelle McGrath, who was last seen leaving a bar in the city of Orlando in the early hours.
Florida has carried out more executions -- seven -- than any other US state so far this year.
Richard Jordan, 79, was convicted and sentenced to death in 1976 for the murder of Edwina Marter, the wife of a bank executive in the town of Gulfport.
He was apprehended when he went to pick up the money.
The execution in Mississippi will be the first in the southern state since December 2022.
The use of nitrogen gas as an execution method has been denounced by United Nations experts as cruel and inhumane.
President Donald Trump is a proponent of capital punishment, and on his first day in office called for an expansion of its use “for the vilest crimes.”
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