Two complexes L(MAcO)(2) (M=Cu, Zn) containing calix[4]arene ligand H2L modified by salicylaldehyde acylhydrazone have been synthesized and characterized by elemental analysis, MS(ESI), IR, UV-vis and fluorescence. Whereas L(ZnAcO)(2) exhibited an enhancement in fluorescence, the potentiality of H2L acting as a Zn2+-selective fluorescence probe was investigated. Results showed that a good linearity (correlation coefficient 0.999) between fluorescence intensity and concentration of Zn2+ in range of 4.0x10(-6) similar to 4.0x10(-5) mol-L-1 existed in H2L solution of 1.0x10(-4) mol.L-1. The minimum concentration at which H2L could detect Zn2+ was 1.0 x10(-6) mol.L-1. Co-existence of Cu2+, Ni2+ and Mn2+ would interfere the determination of Zn2+, but no influence by Na+, me, Cd2+ and Pb2+.