In the present study, we report the synthesis of aqueous stable gold nanoparticles by using calix[4]arene polyhydrazide (CPH) as both reducing and capping agents. The calix[4]arene polyhydrazide reduced gold nanoparticles (CPH-AuNps) were characterized by UV/Vis, particle size analyzer (PSA) and transmission electron mictroscopy (TEM). The records confirmed high stability of CPH-AuNps in aqueous solution over a long period of time and even at varied pH. Additionally, CPH-AuNps have been investigated for its application as "Turn Off" fluorescent sensor for Hg[II]. A concentration of Hg[II] in the limit of 10 nM to 10 microM can be detected based on fluorescence quenching of the CPH-AuNPs and it was also concluded from the spectroscopic data that CPH-AuNPs possess excellent selectivity to Hg[II] over several metal ions like Pb[II], Cu[II], Cd[II], Mn[II], Zn[II] and Ni[II].