A new adsorbent, silicapolyaniline has been synthesized. The material was characterized on the basis of FTIR, XRD and SEM studies. X-ray diffraction study of silica polyaniline reveals mixed crystalline and amorphous phases indicating its semi crystalline nature. The analytical applicability of this newly synthesized material has been established by using it as stationary phase in thin layer chromatographic analysis of nine surfactants (both non-ionic and cationic), amino acids and metal ions with different solvent systems. This material was found useful for the separation of cationic surfactants from non-ionic surfactants with 1.0 M aqueous formic acid or sodium formate solution. However, the separation of L-alanine or L-glycine from L-leuicine or other amino acids could be possible with 1.0 M aqueous formic acid whereas for the separation of metal ions, mixture of 1.0 M aqueous solutions of formic acid and sodium formate in 1:1 volume ratio was most suitable. Ni2+ with higher RF value can be well separated from Hg2+ and Zn2+.