New method for rapid solid-phase extraction of large-volume water samples and its application to non-target screening of North Sea water for organic contaminants by gas chromatography-mass spectrometry.

A method has been developed that allows the solid-phase extraction of microorganic compounds from large volumes of water (10 l) for non-target analysis of filtered seawater. The filtration-extraction system is operated with glass fibre filter candles and the polymeric styrene-divinylbenzene sorbent SDB-1 at flow-rates as high as 500 ml/min. Recovery studies carried out for a couple of model substances covering a wide range of polarity and chemical classes revealed a good performance of the method. Especially for polar compounds (log Kow 3.3-0.7) quantitative recovery was achieved. Limits of detection were between 0.1 and 0.7 ng/l in the full scan mode of the MS. The suitability of the method for the analysis of marine water samples is demonstrated by the non-target screening of water from the German Bight for the presence of organic contaminants. In the course of this screening a large variety of substances was identified including pesticides, industrial chemicals and pharmaceuticals. For some of the identified compounds their occurrence in marine ecosystems has not been reported before, such as dichloropyridines, carbamazepine, propyphenazone and caffeine.

[1]  N. Theobald,et al.  Hydrophobic organic micropollutants in samples of coastal waters: efficiencies of solid-phase extraction in the presence of humic substances , 1998 .

[2]  K. Verschueren.  Handbook of environmental data on organic chemicals , 1977 .

[3]  J. Duinker,et al.  Polychlorinated biphenyls in North Sea water , 1991 .

[4]  W. Specht,et al.  Gas-chromatographische Bestimmung von Rückständen an Pflanzenbehandlungsmitteln nach Clean-up über Gel-Chromatographie und Mini-Kieselgel-Säulen-Chromatographie , 1985 .

[5]  J. Grimalt,et al.  Intercomparison Study of Liquid - Liquid Extraction and Adsorption on Polyurethane and Amberlite XAD , 1988 .

[6]  M. Ehrhardt,et al.  Petroleum-derived dissolved organic compounds concentrated from inshore waters in Bermuda , 1990 .

[7]  Y. Picó,et al.  Spatial and Temporal Trends of Paraquat, Diquat, and Difenzoquat Contamination in Water from Marsh Areas of the Valencian Community (Spain) , 1998, Archives of environmental contamination and toxicology.

[8]  E. Benfenati,et al.  Simultaneous analysis of 50 pesticides in water samples by solid phase extraction and GC-MS , 1990 .

[9]  D. Barceló,et al.  Tracing polar benzene- and naphthalenesulfonates in untreated industrial effluents and water treatment works by ion-pair chromatography-fluorescence and electrospray-mass spectrometry , 1999 .

[10]  F. Renner,et al.  Mass spectrometric investigations of water extracts of the river Elbe for the determination of potential inputs of pollutants into the North Sea , 1995 .

[11]  K. Bester,et al.  Results of non target screening of lipophilic organic pollutants in the German Bight. IV: Identification and quantification of chloronitrobenzenes and dichloronitrobenzenes , 1998 .

[12]  N. Kannan,et al.  Distribution of individual chlorobiphenyls (PCB) in solution and suspension in the Baltic Sea , 1995 .

[13]  M. Waldock,et al.  Concentrations of alkyphenol polyethoxylates entering UK estuaries , 1999 .

[14]  M. Jekel,et al.  Comparison of Sorbents Using Semipolar to Highly Hydrophilic Compounds for a Sequential Solid-Phase Extraction Procedure of Industrial Wastewaters , 1996 .

[15]  S. Kira,et al.  Measurement of a Time-Weighted Average Concentration of Polycyclic Aromatic Hydrocarbons in Aquatic Environment Using Solid Phase Extraction Cartridges and a Portable Pump , 1997, Bulletin of environmental contamination and toxicology.

[16]  H. Gaul,et al.  Method for the analysis of lipophilic compounds in water and results about the distribution of different organochlorine compounds in the North Sea , 1983 .

[17]  N. Paxéus,et al.  Organic pollutants in the effluents of large wastewater treatment plants in Sweden , 1996 .

[18]  D. F. Hagen,et al.  Solid-phase extraction of phenols using membranes loaded with modified polymeric resins , 1993 .

[19]  T. Bidleman,et al.  Analysis of pesticides in seawater after enrichment onto C8 bonded-phase cartridges. , 1989 .

[20]  Y. Picó,et al.  Solid-phase extraction in multi-residue pesticide analysis of water. , 1993, Journal of chromatography.

[21]  A. Hendriks,et al.  Monitoring response of XAD-concentrated water in the rhine delta : a major part of the toxic compounds remains unidentified , 1994 .

[22]  F. Hernández,et al.  Solid-phase extraction of pesticide residues from ground water: comparison between extraction cartridges and extraction discs , 1993 .

[23]  K. Unger,et al.  Analysis of organic pollutants in water at trace levels using fully automated solid-phase extraction coupled to high-performance liquid chromatography , 1997 .

[24]  O. Jáuregui,et al.  Determination of phenols in sea water by liquid chromatography with electrochemical detection after enrichment by using solid-phase extraction cartridges and disks , 1995 .

[25]  John L. Zhou,et al.  Fluxes of organic contaminants from the river catchment into, through and out of the Humber estuary, UK , 1999 .

[26]  J. Clark,et al.  A Rapid Method for the Simultaneous Analysis of Chlorpyrifos, Isofenphos, Carbaryl, Iprodione, and Triadimefon in Groundwater by Solid-Phase Extraction , 1990 .

[27]  A. Noble.  Partition coefficients (n-octanol—water) for pesticides , 1993 .

[28]  G. Font,et al.  Solid-phase extraction of organochlorine pesticides from water samples. , 1990 .

[29]  A. Marcomini,et al.  Graphitized carbon black extraction cartridges for monitoring polar pesticides in water , 1993 .

[30]  G. Durell,et al.  Determining Produced Water Originating Polycyclic Aromatic Hydrocarbons in North Sea Waters: Comparison of Sampling Techniques , 1999 .

[31]  D. Barceló,et al.  Improvements in the determination of organophosphorus pesticides in ground- and wastewater samples from interlaboratory studies by automated on-line liquid-solid extraction followed by liquid chromatography-diode array detection , 1996 .

[32]  T. Ternes,et al.  Simultaneous determination of antiseptics and acidic drugs in sewage and river water , 1998 .

[33]  J. Duinker,et al.  An in-situ filtration/extraction system for the recovery of trace organics in solution and on particles tested in deep ocean water , 1996 .

[34]  D. F. Hagen,et al.  Membrane approach to solid-phase extractions , 1990 .

[35]  J. Richard,et al.  Organics in water: solid phase extraction on a small scale , 1988 .

[36]  S. Franke,et al.  Organic compounds as contaminants of the Elbe River and its tributaries , 1995 .

[37]  R. Niessner,et al.  Analysis of aromatic sulfonates in water by solid-phase extraction and capillary electrophoresis. , 1998, Journal of chromatography. A.

[38]  D. Barceló,et al.  Screening of organophosphorus pesticides in environmental matrices by various gas chromatographic techniques , 1993 .

[39]  M. Hennion,et al.  Simple removal of humic and fulvic acid interferences using polymeric sorbents for the simultaneous solid-phase extraction of polar acidic, neutral and basic pesticides , 1996 .

[40]  J. Readman,et al.  Comparison of the performance of solid-phase extraction techniques in recovering organophosphorus and organochlorine compounds from water , 1996 .

[41]  D. Barceló,et al.  Monitoring of pesticides in river water based on samples previously stored in polymeric cartridges followed by on-line solid-phase extraction-liquid chromatography–diode array detection and confirmation by atmospheric pressure chemical ionization mass spectrometry , 1999 .

[42]  A. Di Corcia,et al.  Multiresidue method for pesticides in drinking water using a graphitized carbon black cartridge extraction and liquid chromatographic analysis. , 1991, Analytical chemistry.

[43]  D. Barceló,et al.  Solid-phase sample preparation and stability of pesticides in water using Empore disks , 1994 .

[44]  D. Barceló,et al.  On-line and off-line sample preparation of acidic herbicides and bentazone transformation products in estuarine waters , 1994 .

[45]  U. Brinkman,et al.  Analysis of microcontaminants in aqueous samples by fully automated on-line solid-phase extraction-gas chromatography-mass selective detection , 1996 .