Sucralose screening in European surface waters using a solid-phase extraction-liquid chromatography-triple quadrupole mass spectrometry method.

An analytical method was developed for the analysis of sucralose, a persistent chlorinated calorie-free sugar substitute, in surface waters. The method is based on solid-phase extraction (SPE) of 400mL water using Oasis HLB (Waters) adsorber material, followed by negative electrospray ionization (ESI) triple quadrupole LC-MS-MS detection. Quantification was performed by external calibration, as well as by isotope dilution with deuterated sucralose d6 internal standard. Extraction with Oasis HLB, a polymeric adsorbent suited for polar compounds, was much more efficient at neutral pH than at pH 3; a recovery of 62+/-9% (n=6; determined at 1microg/L) could be achieved. Strong ion suppression caused by matrix substances was observed for sucralose in the SPE extracts. The analysis of 120 river surface water samples from 27 European countries showed that sucralose, which is in use in Europe since beginning 2005, can be found in the aquatic environment, at concentrations up to 1microg/L. Sucralose was predominately found in samples from the UK, Belgium, the Netherlands, France, Switzerland, Spain, Italy, Norway, and Sweden, suggesting an increased use of the substance in Western Europe.

Occurrence of polar organic contaminants in the dissolved water phase of the Danube River and its major tributaries using SPE-LC-MS(2) analysis.

Polar water-soluble organic contaminants were analysed in the dissolved liquid water phase of river water samples from the Danube River and its major tributaries (within the Joint Danube Survey 2). Analyses were performed by solid-phase extraction (SPE) followed by triple-quadrupole liquid chromatography mass spectrometry (LC-MS(2)). In total, 34 different polar organic compounds were screened. Focus was given on pharmaceutical compounds (such as ibuprofen, diclofenac, sulfamethoxazole, carbamazepine), pesticides and their degradation products (e.g. bentazone, 2,4-D, mecoprop, atrazine, terbutylazine, desethylterbutylazine), perfluorinated acids (PFOS; PFOA), and endocrine disrupting compounds (nonylphenol, NPE(1)C, bisphenol A, estrone). The most relevant polar compounds identified in the Danube River basin in terms of frequency of detection, persistency, and concentration levels were 1H-benzotriazole (median concentration 185 ng/L), caffeine (87 ng/L), tolyltriazole (73 ng/L), nonylphenoxy acetic acid (49 ng/L), carbamazepine (33 ng/L), 4-nitrophenol (29 ng/L), 2,4-dinitrophenol (19 ng/L), PFOA (17 ng/L), sulfamethoxazole (16 ng/L), desethylatrazine (11 ng/L), and 2,4-D (10 ng/L). The highest contamination levels were found in the area around Budapest and in the tributary rivers Arges (Romania), Timok (Bulgaria), Rusenski Lom (Bulgaria), and Velika Morava (Serbia).

Pan-European survey on the occurrence of selected polar organic persistent pollutants in ground water.

This study provides the first pan-European reconnaissance of the occurrence of polar organic persistent pollutants in European ground water. In total, 164 individual ground-water samples from 23 European Countries were collected and analysed (among others) for 59 selected organic compounds, comprising pharmaceuticals, antibiotics, pesticides (and their transformation products), perfluorinated acids (PFAs), benzotriazoles, hormones, alkylphenolics (endocrine disrupters), Caffeine, Diethyltoluamide (DEET), and Triclosan. The most relevant compounds in terms of frequency of detection and maximum concentrations detected were DEET (84%; 454 ng/L), Caffeine (83%; 189 ng/L), PFOA (66%; 39 ng/L), Atrazine (56%; 253 ng/L), Desethylatrazine (55%; 487 ng/L), 1H-Benzotriazole (53%; 1032 ng/L), Methylbenzotriazole (52%; 516 ng/L), Desethylterbutylazine (49%; 266 ng/L), PFOS (48%, 135 ng/L), Simazine (43%; 127 ng/L), Carbamazepine (42%; 390 ng/L), nonylphenoxy acetic acid (NPE(1)C) (42%; 11 microg/L), Bisphenol A (40%; 2.3 microg/L), PFHxS (35%; 19 ng/L), Terbutylazine (34%; 716 ng/L), Bentazone (32%; 11 microg/L), Propazine (32%; 25 ng/L), PFHpA (30%; 21 ng/L), 2,4-Dinitrophenol (29%; 122 ng/L), Diuron (29%; 279 ng/L), and Sulfamethoxazole (24%; 38 ng/L). The chemicals which were detected most frequently above the European ground water quality standard for pesticides of 0.1 microg/L were Chloridazon-desphenyl (26 samples), NPE(1)C (20), Bisphenol A (12), Benzotriazole (8), N,N'-Dimethylsulfamid (DMS) (8), Desethylatrazine (6), Nonylphenol (6), Chloridazon-methyldesphenyl (6), Methylbenzotriazole (5), Carbamazepine (4), and Bentazone (4). However, only 1.7% of all single analytical measurements (in total 8000) were above this threshold value of 0.1 microg/L; 7.3% were > than 10 ng/L.

EU-wide survey of polar organic persistent pollutants in European river waters.

This study provides the first EU-wide reconnaissance of the occurrence of polar organic persistent pollutants in European river waters. More than 100 individual water samples from over 100 European rivers from 27 European Countries were analysed for 35 selected compounds, comprising pharmaceuticals, pesticides, PFOS, PFOA, benzotriazoles, hormones, and endocrine disrupters. Around 40 laboratories participated in this sampling exercise. The most frequently and at the highest concentration levels detected compounds were benzotriazole, caffeine, carbamazepine, tolyltriazole, and nonylphenoxy acetic acid (NPE(1)C). Only about 10% of the river water samples analysed could be classified as "very clean" in terms of chemical pollution. The rivers responsible for the major aqueous emissions of PFOS and PFOA from the European Continent could be identified. For the target compounds chosen, we are proposing "indicative warning levels" in surface waters, which are (for most compounds) close to the 90th percentile of all water samples analysed.