The electrospray (ES) behaviour of selected Remazol textile dyes, their hydrolysis products and the latters' reaction, following elution from a strong anion-exchange cartridge, with 30% concentrated HCl in MeOH, is studied and applied to the direct analysis of dye containing effluent. For unambiguous identification and determination of these textile dyes in effluents, it is necessary to resort to ES utilising MS-MS and MS3. Further, a tabular review of recent applications of HPLC-ES-MS and, to a lesser extent, CE-ES-MS with reference to drug and pesticide analysis is presented.