Emerging contaminant determination in water samples by liquid chromatography using a monolithic column coupled with a photodiode array detector

摘要

Concern about the presence of emerging contaminants in the environment has increased because biological activity at low concentrations has been observed. The difficulty of detecting and quantifying these compounds encourages the development of analytical methods with highly sensitive and selective analytical procedures. Pharmaceuticals, pesticides, and industrial chemicals are used and finally discarded to the environment. This paper provides a rapid and sensitive analytical method for the quantification of eight emerging contaminants (carbamazepine, carbofuran, bisphenol A, diuron, 17 alpha ethinylestradiol, ametryn, carbazole, and triclosan). A two-level full factorial design for optimization of chromatographic separation and sample preparation was performed. The separation using a monolithic column (Onyx C18) achieved baseline resolution for all compounds in 4.6 min. The optimized sample treatment involved a preconcentration step by means of solid-phase extraction using HF Bond Elut-C18 cartridges, achieving an enrichment factor of 2222. Under optimum conditions, good linearity was obtained with a correlation coefficient higher than 0.999. The limits of detection and quantification for carbamazepine, carbofuran, bisphenol A, diuron, 17 alpha ethinylestradiol, ametryn, and carbazole were in the range of 0.01-208.7 and 0.03-695.7 ng L-1, respectively, and for triclosan, the limit of detection and quantification was 0.67 and 2.25 mu g L-1, respectively. Precision evaluated as relative standard deviations was lower than 15 . The proposed method was found robust. Finally, the method was successfully applied to superficial water samples.