The creation of smart materials is a current goal of many laboratories including our own. We are involved in studying a number of thin film and monolayer systems which share the common features of involving highly conjugated conducting organic polymers and the evolved properties of specific biological macromolecules. In this report we describe a generic ‘cassette’ methodology for immobilizing biotinylated biological macromolecules to hydrophobic surfaces using a novel class of conducting copolymers of polythiophene. These copolymers are derivatized with long alkyl chains and biotin moieties to bind, respectively, to the hydrophobic surface and the biotinylated species, through the biotin - streptavidin interaction. We utilize the monolayer ‘cassette’ approach to attach a signal transducing biomolecule alkaline phosphatase to the surface of a glass capillary. This produces a flexible system in which chemiluminescence provides the basis for a useful measurement strategy. A novel technique involving the generation of chemiluminescence signal from alkaline phosphatase catalyzed dephosphorylation of a macrocyclic phosphate compound is described. Detection of paraoxon and methyl parathion, both enzyme inhibitors, has been achieved at ppb levels. The technique is rapid, sensitive, and is applicable to the detection of all organophosphorus based insecticides. The technique will be used in developing a fiber;optic biosensor for remote detection of insecticides.