High sensitive multiresidue analysis of pharmaceuticals and antifungals in surface water using U-HPLC-Q-Exactive Orbitrap HRMS. Application to the Danube river basin on the Romanian territory

Science of the Total Environment

Volumn 532, Issue , 2015, Pages 501-511

  Chitescu, Carmen Lidia ^a   Kaklamanos, George ^b   Nicolau, Anca Ioana ^a   Stolker, Alida Adriana Maria Linda ^b  

^a DUNAREA DE JOS UNIVERSITY OF GALATI   (Romania)

^b WAGENINGEN UNIVERSITY   (Netherlands)

Author keywords

Antifungals; Danube river; High resolution; Orbitrap; Pharmaceutical residues

Indexed keywords

AMIDES; PHASE SEPARATION; RECOVERY; RIVERS; SURFACE WATERS;

ANTIFUNGALS; DANUBE RIVERS; HIGH RESOLUTION; ORBITRAP; PHARMACEUTICAL RESIDUES;

EXTRACTION;

ANTIFUNGAL AGENT; CARAZOLOL; CARBAMAZEPINE; CARBENDAZIM; CHLORAMPHENICOL; CIPROFLOXACIN; DICLOFENAC; DICLOXACILLIN; DOXYCYCLINE; DRUG RESIDUE; ENILCONAZOLE; EPOXICONAZOLE; FLUBENDAZOLE; INDOMETACIN; ITRACONAZOLE; KETOPROFEN; LINCOMYCIN; NAPROXEN; OXYTETRACYCLINE; PIROXICAM; PRAZIQUANTEL; SALINOMYCIN; SULFAMETHOXAZOLE; SURFACE WATER; TEBUCONAZOLE; TIABENDAZOLE; TIAMULIN; TILMICOSIN; TYLOSIN; DRUG; WATER POLLUTANT;

CONCENTRATION (COMPOSITION); DRUG; RIVER WATER; TRIBUTARY; WATER CHEMISTRY; WATER QUALITY;

ANALYTIC METHOD; ARTICLE; CONCENTRATION (PARAMETERS); CONTROLLED STUDY; GEOGRAPHIC DISTRIBUTION; HIGH PERFORMANCE LIQUID CHROMATOGRAPHY; LIMIT OF DETECTION; LIMIT OF QUANTITATION; MASS SPECTROMETRY; MEASUREMENT ACCURACY; MEASUREMENT PRECISION; MEASUREMENT REPEATABILITY; PRIORITY JOURNAL; RESIDUE ANALYSIS; RIVER BASIN; ROMANIA; SEASONAL VARIATION; SENSITIVITY ANALYSIS; SOLID PHASE EXTRACTION; TANDEM MASS SPECTROMETRY; WATER ANALYSIS; WATER QUALITY; WATER SAMPLING; ANALYSIS; CHEMISTRY; ENVIRONMENTAL MONITORING; LIQUID CHROMATOGRAPHY; PROCEDURES; RIVER; WATER POLLUTANT;

DANUBE RIVER; ROMANIA;

CARBAMAZEPINE; CHROMATOGRAPHY, HIGH PRESSURE LIQUID; CHROMATOGRAPHY, LIQUID; DICLOFENAC; ENVIRONMENTAL MONITORING; KETOPROFEN; PHARMACEUTICAL PREPARATIONS; RIVERS; ROMANIA; SOLID PHASE EXTRACTION; SULFAMETHOXAZOLE; TANDEM MASS SPECTROMETRY; WATER POLLUTANTS, CHEMICAL;

EID: 84935011486     PISSN: 00489697     EISSN: 18791026     Source Type: Journal    
DOI: 10.1016/j.scitotenv.2015.06.010     Document Type: Article

References (53)

1. Abuin S., Codony R., Compano R., Granados M., Prat M.D. Analysis of macrolide antibiotics in river water by solid-phase extraction and liquid chromatography-mass spectrometry. J. Chromatogr. A 2006, 1114:73-81.
2. Ajeagah G.A., Cioroi M., Praisler M., Constantin O., Palela M., Bahrim G. An ecological assessment of the pollution status of the Danube River Basin in the Galati Region-Romania. J. Water Resour. Prot. 2013, 5:876-886.
3. Arnold K.E., Boxall A.B.A., Brown A.R., Cuthbert R.J., Gaw S., Hutchinson T.H., et al. Assessing the exposure risk and impacts of pharmaceuticals in the environment on individuals and ecosystems. Biol. Lett. 2013, 10.1098/rsbl.2013.0492.
4. Berendsen B., Pikkemaat M., Römkens P., Wegh R., Van Sisseren M., Stolker L., Nielen M.J. Occurrence of chloramphenicol in crops through natural production by bacteria in soil. Agric. Food Chem. 2013, 61(17):4004-4010.
5. Bottoni P., Caroli S. Detection and quantification of residues and metabolites of medicinal products in environmental compartments, food commodities and workplaces. A review. J. Pharm. Biomed. Anal. 2015, 106:3-24.
6. Bottoni P., Carolib S., Barra-Caracciolo A. Pharmaceuticals as priority water contaminants. Toxicol. Environ. Chem. 2010, 3:549-565.
7. Bourdat-Deschamps M., Leang S., Bernet N., Daudin J.J., Nélieu S. Multi-residue analysis of pharmaceuticals in aqueous environmental samples by online solid-phase extraction-ultra-high-performance liquid chromatography-tandem mass spectrometry: optimisation and matrix effects reduction by quick, easy, cheap, effective, rugged and safe extraction. J. Chromatogr. A 2014, 1349:11-23.
8. Boxall A.B.A., Blankwell P., Calallo R., Kong P., Tolls J. The sorption and transport of sulphonamide antibiotics in soil systems. Toxicol. Lett. 2002, 131:19-28.
9. Brooks B.W., Chambliss C.K., Stanley J.K., Ramirez A., Banks K.E., Johnson R.D., Lewis R.J. Determination of select antidepressants in fish from an effluent-dominated stream. Environ. Toxicol. Chem. 2005, 24(2):464-469.
10. Chitescu C.L., Oosterink E., de Jong J., Stolker A.A.M. Accurate mass screening of pharmaceuticals and fungicides in water, by U-HPLC. Anal. Bioanal. Chem. 2012, 403:2997-3011.
11. Commission Decision 2002/657/EC, implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results. Off. J. Eur. Commun. 2002, L221:8-36.
12. Cooper K.M., McMahon C., Fairweather I., Elliott C.T. Potential impacts of climate change on veterinary medicinal residues in livestock produce: an island of Ireland perspective. Trends Food Sci. Technol. 2014, 1-15. 10.1016/j.tifs.2014.03.007.
13. Council Directive 96/23/EC, on measures to monitor certain substances and residues thereof in live animals and animal products and repealing Directives 85/358/EEC and 86/469/EEC and Decisions 89/187/EEC and 91/664/EEC. Off. J. Eur. Commun. 1996, L125:10-32.
14. Danube River Protection Convention (accessed February 2015). http://www.icpdr.org/main/.
15. Directive 2000/60/EC of October 23, 2000 establishing a framework for community action in the field of water policy. O.J. L 327, December 22 2000.
16. Directive 2001/82/EC of the European Parliament and of the Council of 6 November 2001 on the Community code relating to veterinary medicinal products. OJ L 311 2001, 1-66. (28 November).
17. Directive 2001/83/EC of the European Parliament and of the Council of 6 November 2001 on the community code relating to medicinal products for human use. OJ L 311 2001, 67. (28 November).
18. Directive 2013/39/EU of the European Parliament and of the Council of 12 August 2013 amending Directives 2000/60/EC and 2008/105/EC as regards priority substances in the field of water policy. O.J. L 226/1 2013, (24 August).
19. European Environment Agency Pharmaceuticals in the environment. Technical Report No 1/2010 2010, 4. (available at: www.eea.europa.eu/publications/pharmaceuticals-in-the-environment-result-of-an-eea-workshop/at_download/file (accessed February 2015)).
20. Fedorova G., Randok T., Lindberg R.H., Grabic R. Comparison of the quantitative performance of a Q-Exactive high-resolution mass spectrometer with that of a triple quadrupole tandem mass spectrometer for the analysis of illicit drugs in wastewater. Rapid Commun. Mass Spectrom. 2013, 27(15):1751-1762.
21. Fedorova G., Randak T., Golovko O., Kodes V., Grabicova K., Grabic R. A passive sampling method for detecting analgesics, psycholeptics, antidepressants and illicit drugs in aquatic environments in the Czech Republic. Sci. Total Environ. 2014, 487:681-687. (Jul 15).
22. Ferrari F., Gallipoli A., Balderacchi M., Ulaszewska M.M., Capri E., Trevisa M. Exposure of the main Italian river basin to pharmaceuticals. J. Toxicol. 2011, 10.1155/2011/989270.
23. García-Galán M.J., Díaz-Cruz M.S., Barceló D. Occurrence of sulfonamide residues along the Ebro river basin: removal in wastewater treatment plants and environmental impact assessment. Environ. Int. 2011, 37(2):462-473.
24. Gros M., Petrovic M., Barceló D. Data set on the occurrence of pharmaceutical compounds in the samples from the Danube river basin. AquaTerra report. Project no. 505428 (GOCE) 2006.
25. Gros M., Rodríguez-Mozaz S., Barceló D. Fast and comprehensive multi-residue analysis of a broad range of human and veterinary pharmaceuticals and some of their metabolites in surface and treated waters by ultra-high-performance liquid chromatography coupled to quadrupole-linear ion trap tandem mass spectrometry. J. Chromatogr. A 2012, 1248:104-121.
26. Gunnarsson L., Jauhiainen A., Kristiansson E., Nerman O., Larsson D.G.J. Evolutionary conservation of human drug targets in organisms used for environmental risk assessments. Environ. Sci. Technol. 2008, 42(15):5807-5813.
27. Heuett N.V., Ramirez C.E., Fernandez A., Gardinali P.R. Analysis of drugs of abuse by online SPE-LC high resolution mass spectrometry: communal assessment of consumption. Sci. Total Environ. 2015, 511:319-330.
28. Huang C.H., Renew J.E., Smeby K.L., Pinkston K., Sedlak D.L. Assessment of potential antibiotic contaminants in water and preliminary occurrence analysis. J. Contemp. Water Res. Educ. 2001, 120:30-40.
29. ICH Validation of Analytical Procedures: Text and Methodology Q2(R1), International Conference on Harmonization available on;, (Accessed Nov 2014). http://www.ich.org/products/guidelines/quality/quality-single/article/validation-of-analytical-procedures-text-and-methodology.html.
30. Iglesias A., Nebot C., Vázquez B.I., Miranda J.M., Abuín F., Cepeda A. Detection of veterinary drug residues in surface waters collected nearby farming areas in Galicia, north of Spain. Environ. Sci. Pollut. Res. 2014, 21(3):2367-2377.
31. Joint Danube Survey (JDS) 3-2013 A Comprehensive Analysis of Danube Water Quality. Final Report 2015, International Commission for the Protection of the Danube River, Vienna.
32. Kosjek T., Heath E. Applications of mass spectrometry to identifying pharmaceutical transformation products in water treatment. Trends Anal. Chem. 2008, 27(10):807-820.
33. Kümmerer K. Pharmaceuticals in the environment. Annu. Rev. Environ. Resour. 2010, 35:57-75.
34. Mackuľak T., Skubák J., Grabic R., Ryba J., Birošová L., Fedorova G., Spalková V., Bodík I. National study of illicit drug use in Slovakia based on wastewater analysis. Sci. Total Environ. 2014, 494-495:158-165.
35. Madureira T., Barreiro J., Rocha M., Cass Q., Tiritan M. Spatio-temporal distribution of pharmaceuticals in the Douro River estuary (Portugal). Sci. Total Environ. 2010, 408(22):5513-5520.
36. Marín J.M., Gracia-Lor E., Sancho J.V., López F.J., Hernández F. Application of ultra-high-pressure liquid chromatography-tandem mass spectrometry to the determination of multi-class pesticides in environmental and wastewater samples: study of matrix effects. J. Chromatogr. A 2009, 1216(9):1410-1420.
37. Marti E., Variatza E., Balcaza J.L. The role of aquatic ecosystems as reservoirs of antibiotic resistance. Trends Microbiol. 2014, 22:36-41.
38. Meredith-Williams M., Carter L.J., Fussell R., Raffaelli D., Ashauer R., Boxall A.B.A. Uptake and depuration of pharmaceuticals in aquatic invertebrates. Environ. Pollut. 2012, 165:250-258.
39. Petrović M., Škrbić B., Živančev J., Ferrando-Climent L., Barcelo D. Determination of 81 pharmaceutical drugs by high performance liquid chromatography coupled to mass spectrometry with hybrid triple quadrupole-linear ion trap in different types of water in Serbia. Sci. Total Environ. 2014, 468-469:415-428.
40. Rabolle M., Spliid N.H. Sorption and mobility of metronidazole, olaquindox, oxytetracycline and tylosin in soil. Chemosphere 2000, 40:715-722.
41. Ramirez A.J., Brain R.A., Usenko S., Mottaleb M.A., O'Donnell J.G., Stahl L.L., et al. Occurrence of pharmaceuticals and personal care products (PPCPs) in fish: results of a national pilot study in the U.S. Environ. Toxicol. Chem. 2009, 28(12):2587-2597.
42. RED Facts - Environmental Protection Agency Report Number, EPA/738/F-05/001. Environmental Protection And Toxic Substances March, (accessed February 2015). http://www.epa.gov/opp00001/reregistration/REDs/factsheets/0196fact.pdf.
43. Rivera Z.H., Oosterink E., Rietveld L., Schoutsen F., Stolker A.A.M. Influence of natural organic matter on the screening of pharmaceuticals in water by using liquid chromatography with full scan mass spectrometry. Anal. Chim. Acta 2011, 700:114-125.
44. Santos I.J.S., Grossman M.J., Sartoratto A., Ponezi A.N., Durrant L.R. Degradation of the recalcitrant pharmaceuticals carbamazepine and 17α-ethinylestradiol by ligninolytic fungi. Chem. Eng. Trans. 2012, 27:169-174.
45. Solliec M., Roy-Lachapelle A., Sauvé S. Quantitative performance of liquid chromatography coupled to Q-Exactive high resolution mass spectrometry (HRMS) for the analysis of tetracyclines in a complex matrix. Anal. Chim. Acta 2015, 853:415-424.
46. Ter Laak T., van der Aa M., Houtman C., Stoks P., van Wezel A. Temporal and Spatial Trends of Pharmaceuticals in the Rhine 2010, Association of River Waterworks - RIWA-Rhine, The Netherlands, (February).
47. The Danube Delta - A Biosphere Reserve Authority (accessed March 2015). http://www.ddbra.ro/en/danube-delta-biosphere-reserve/danube-delta/general-presentation/danube-delta-a1049.
48. Tiehm A., Schmidt N., Stieber M., Sacher F., Wolf L., Hoetzl H. Biodegradation of pharmaceutical compounds and their occurrence in the Jordan Valley. Water Resour. Manag. 2011, 25:1195-1203.
49. Tolls J. Sorption of veterinary pharmaceuticals in soils: a review. Environ. Sci. Technol. 2001, 35:3397-3406.
50. Van der Heeft E., Bolck Y.J.C., Beumer B., Nijrolder A.W.J.M., Stolker A.A.M., Nielen M.W.F. Full-scan accurate mass selectivity of ultra-performance liquid chromatography combined with time-of-flight and orbitrap mass spectrometry in hormone and veterinary drug residue analysis. J. Am. Soc. Mass Spectrom. 2009, 20:451-463.
51. Vázquez M.M., Vázquez P.P., Galera M.M., García M.D. Determination of eight fluoroquinolones in groundwater samples with ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction prior to high-performance liquid chromatography and fluorescence detection. Anal. Chim. Acta 2012, 748:20-27.
52. Vazquez-Roig P., Andreu V., Onghena M., Blasco C., Picó Y. Assessment of the occurrence and distribution of pharmaceuticals in a Mediterranean wetland (L'Albufera, Valencia, Spain) by LC-MS/MS. Anal. Bioanal. Chem. 2011, 400:1287-1301.
53. Wang J., Gardinali P.R. Identification of phase II pharmaceutical metabolites in reclaimed water using high resolution benchtop Orbitrap mass spectrometry. Chemosphere 2014, 107:65-73.