New molecular azo-azomethine receptor, HL, was synthesized via condensation reaction of 2-hydroxy-3-methoxy-5-((2,4-dichlorophenyl)diazenyl)benzaldehyde with 3-aminopropyl triethoxysilane (3-APTES) in EtOH. HL was characterized using standard spectroscopic techniques (FT-IR, 1H NMR and UV-Vis). The sensing ability of HL was investigated towards the inorganic anions in DMSO and DMSO/H2O (1:4 v/v) media. Also, new azo-azomethine receptor immobilized in MCM-41, S-MCM, has been prepared by reaction of amino-modified MCM-41 support with 2-hydroxy-3-methoxy-5-((2,4-dichlorophenyl)diazenyl)benzaldehyde in anhydrous EtOH. The mesoporous hybrid material, S-MCM, was characterized by elemental analysis, Fourier-transform infrared spectra, powder X-ray diffraction (XRD), scanning electron microscopy (SEM), and nitrogen (N2) adsorption–desorption (BET). S-MCM was applied for detection of anions in aqueous and semi-aqueous media.[1,2]