This paper describes a novel aerosol chemiluminescencebaseddetector, which can be coupled to liquid chromatographyfor the determination of the chemicals with weakoptical absorbance in the UV-visible region. This aerosolchemiluminescence (CL)-based detector, in which HPLCeffluent is converted to aerosol and then generated CLemission on the surface of porous alumina, is composedof three main processes: nebuliztion of HPLC effluent, CL emission on surface of porous alumina material, andoptical detection. To demonstrate the utility of the aerosolchemiluminescence detector, some compounds such saccharides, poly (ethylene glycol)s, amino acids, and steroidpharmaceuticals are determined by the present aerosolchemiluminescence detection method. Compared with anevaporative light scattering detector, the proposed detectorshows the following features: (a) extensive CL emissionson porous alumina by many compounds tested, which leads to the potential application for the determinationof volatile and nonvolatile chemicals with or withoutUV-visible absorbance; (b) a CL mechanism based on thecatalytic oxidation of analytes, not on the light scattering,which suggests the present detector be free from theinterference of the inorganic and nonvolatile mobile-phasemodifiers. The CL characteristics and effect of differentparameters, such as temperature and nebulizer gas flowrate, were also discussed in this paper. Furthermore, thisaerosol chemiluminescence-based detector was successfullyapplied to the determination of raffinose, glucose,sucrose, maltose, and r-lactose.