This invention relates to a method of analytical detection of polycyclic aromatic hydrocarbon and their derivatives in samples. 1,3-Di-naphthalimide conjugate of calix[4]arene is titrated by fluorescence with the said samples and the emission band of the spectra analysed to assess the polycyclic aromatic hydrocarbons contents therein.This invention also includes a novel process for synthesizing 1,3-Di naphthalimide conjugate of calix [4] arene