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The present study describes the monitoring of some of the major classes of surfactants in water. The separation, identification, and the quantitative estimation of the compounds were achieved using LC-Q-ToF-MS. The analyses revealed the presence of variety of surfactants including linear alkylbenzene sulfonate (LAS), alcohol ethoxysulfates (AES), and alcohol ethoxylates (AE). Further, emphasis was given to AES as they are one of the most produced and consumed surfactants in the world. And as far as India is concerned, the present study is one of the most significant attempt regarding the identification and quantification of AES. The data obtained during the analysis revealed that the average concentration of AES C12Ex varied from 0.7 to 13.6 μg L−1 while that of C14Ex ranged between 1.3 and 10.4 μg L−1. The risk assessment revealed that higher chain AES are capable of posing medium level risk to the aquatic compartment. In addition, the study also included the physicochemical analysis of water from the selected area. Water was found to be acidic in nature and the salinity, TDS, and EC values were found to be high during the pre-monsoon season. The order of the levels of anionic constituents was of Cl−>SO42−SO42−>F−>NO32− ≅ PO42− while that of cations were Na+ > Mg2+ > K+ > Ca2+. Results of correlation analysis showed that statistically negative correlation exists between AES homologs and pH while slight positive correlations were found between AES and other parameters including TDS and EC. The suitability of this water for domestic and agricultural purposes has been examined on the ground of basic quality indices such as the water quality index (WQI) and sodium adsorption ratio (SAR). The WQI measurements also revealed that the water quality of the region falls under the “very poor” category especially during the pre-monsoon season. The study could explore the cumulative share of these canals in the quality impairment of the receiving Vembanad Lake. [ABSTRACT FROM AUTHOR]