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ANALYSIS OF PHARMACEUTICAL COMPOUNDS IN WATER BY SPE-UPLC-ESI-MS/MS. A method was developed for the analysis of 31 pharmaceutical compounds in Lisbon's drinking water system, using solid-phase extraction (SPE) and ultraperformance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS). The method was validated through estimation of the linearity range, method detection and quantification limits, matrix effects, precision and accuracy. The method detection and quantification limit ranges were 0.009-10 and 0.03-33 ng/L, respectively. Analytes were quantified in water samples collected from the EPAL (Empresa Portuguesa das Águas Livres S.A.) supply system. Carbamazepine, atenolol, sulfadiazine, sulfamethazine, sulfapyridine, sulfamethoxazole, acetaminophen, caffeine and erythromycin were quantified in the analysed samples.

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The aim of this study was developed and validated an analytical method based on liquid chromatography and tandem mass spectrometry after solid phase extraction to monitorizing ten endocrine hormone disrupters in Lisbon drinking water system. Natural and synthetic hormones (17-β-estradiol, ethinylestradiol, estriol, estrone, progesterone, mestranol and diethylstilbestrol) and some industrial products (4-n-nonylphenol, 4-tert-octylphenol and bisphenol A) were studied. Mass spectrometer detection parameters were optimized, such as the best conditions for the precursor ion formation, namely cone voltage, when applying negative and positive electrospray ionization, and also collision energy for MRM1 and MRM2 transitions. The best conditions of the solid phase extraction (SPE) using Waters Oasis HLB (6 mL, 200 mg) and Isolute C18 (EC) (6 ml, 1000 mg) were also optimized. The method was validated through the application of several statistical tests and the uncertainty estimation of the analytical assay. This method showed a very good linear range for all the studied analytes with determination coefficients (r 2 ) between 0.9962 and 0.9999 and coefficients of variation lower than 4%. There were no significant differences between recoveries obtained with the studied matrices, like groundwater, surface water and water for human consumption. In these matrices, the recovery values varied between 32 and 95%. The limits of method detection were between 0.28 and 22 ng/L. The validated method was applied for the analysis of water samples from the EPAL (Empresa Portuguesa das Águas Livres, S.A.) water supply system including tap water, spring water, groundwater, and river water. Some target compounds (bisphenol A, progesterone, 4-tert-octylphenol, and 4-n-nonylphenol) were found in trace amounts in analysed waters.

a b s t r a c tA multi-barrier system was studied for the production of drinking water with high chemical and microbiological quality. The integration of nanofiltration (NF) and ultraviolet (UV) photolysis was tested at pilot scale in a surface water treatment plant.The NF membranes tested, Desal DK and NF270, allow for the production of permeates with high quality standards, although the membrane with higher molecular weight cut-off (NF270) revealed to be the best option for surface water treatment due to its higher permeability. The NF270 membrane was also efficient to deliver high quality water, even under high pollutant concentrations, making possible to operate with water recovery rates as high as 98%.Extensive studies were performed in the water treatment plant where the proposed system was tested at three locations of the drinking water production line. Seeking to achieve the best compromise between high recovery rate, high retention of chemicals and microorganisms as well as preventing operational problems (flux decline and fouling), it was found that the integrated system should be placed after the conventional sand filtration, operating at a 91% recovery rate. Under the selected conditions -TMP of 8 bar and recovery rate of 91% -it is possible to operate at constant permeability without flux decline for a period of 15 days, after which a gentle CIP procedure is recommended.Membrane fouling was also investigated and the major foulant classes identified were proteins, polysaccharides and humic acids. A cleaning protocol was also tested and the impact of each cleaning step on the recovery of permeability evaluated.