Abstract
A new extraction technique, fluidized-bed extraction, has been investigated for isolation of organochlorine pesticides from sediment. The extraction was optimized, by means of a surface-response design, by considering the number of extraction cycles, the holding time after reaching the heating temperature, and the composition of the extraction solvent as experimental variables. The effect on method performance of the operating conditions used for fluidized-bed extraction was investigated. Special emphasis was given to accurate determination of p,p′-DDT, because DDT is known to be unstable during GC injection. To evaluate the extent of degradation of DDT, 13C12-p,p′-DDT-solutions were analyzed and the amount of degradation during GC injection was calculated. 13C12-p,p′-DDT was also added to sediment samples before extraction and the extent of degradation during the optimization experiment was investigated. Finally, classical Soxhlet extraction was compared with the optimized fluidized-bed extraction method.
This is a preview of subscription content, log in via an institution to check access.
Similar content being viewed by others
References
Bhattacharya B, Sarkar SK, Mukherjee N (2003) Environ Int 29:587–592; DOI 10.1016/s0160–4120(03)00016–3
Fatoki OS, Awofolu RO (2003) J Chromatogr A 983:225–236
Doong R-A, Sun Y-C, Liao P-L, Peng C-K, Wu S-C (2002) Chemosphere 48:237–246
Kim J-H, Smith A (2001) Chemosphere 43:137–140
Barceló D (1991) Analyst 116:681–689
Kucklick JR, Struntz WDJ, Becker PR, York GW, O’Hara TM, Bohonowych JE (2002) Sci Total Environ 287:45–59
Bressa G, Sisti E, Cima F (1997) Mar Chem 58:261–266
Manirakiza P, Covaci A, Nizigiymana L, Ntakimazi G, Schepens P (2002) Environ Pollut 117:447–455
Burke ER, Holden AJ, Shaw IC (2003) Chemosphere 50:529–535
Stuetz W, Prapamontol T, Erhardt JG, Classen HG (2001) Sci Total Environ 273:53–60
Ahmed SA (2000) Toxicology 150:191–206
Mendes JJA (2002) Food Chem Toxicology 40:781–788
Rhind SM (2002) Domest Anim Endocrinol 23:179–187
Dean JR (1998) Extraction methods for environmental analysis. Wiley, Chichester
Dean JR, Wade G (2000) Trends Anal Chem 19:553–564
Barceló D (2000) Sample handling and trace analysis of pollutants—techniques, applications and quality assurance, Elsevier, Amsterdam
Barriada-Pereira M, Concha-Graña E, González-Castro MJ, Muniategui-Lorenzo S, López-Mahía P, Prada-Rodríguez D, Fernández-Fernández E (2003) J Chromatogr A 1008:115–122
Xiong G, He X, Zhang Z (2000) Anal Chim Acta 413:49–56
Lopez-Avila V (1999) Crit Rev Anal Chem 29:95–230
Llompart MP, Lorenzo RA, Cela R, Li K, Bélanger JMR, Paré JRJ (1997) J Chromatogr A 774:243–251
Concha-Grana E, Barriada-Pereira M, Turnes-Carou MI, Muniategui-Lorenzo S, Lopez-Mahia P, Rodriguez DP (2003) Anal Bioanal Chem 375:1225–1228
Silgoner I, Krska R, Lombas E, Gans O, Rosenberg E, Grasserbauer M (1998) Fresenius J Anal Chem 362:120–124
Ramil Criado M, Rodríguez Pereiro I, Cela Torrijos R (2003) J Chromatogr A 985:137–145
Berset JD, Holzer R (1999) J Chromatogr A 852:545–558
Zuin VG, Yariwake JH, Bicchi C (2003) J Chromatogr A 985:159–166
Popp P, Keil P, Möder M, Paschke A, Thuss U (1997) J Chromatogr A 774:203–211
Zhuang W, McKague B, Reeve D, Carey J (2004) Chemosphere 54:467–480; DOI 10.1016/j.chemosphere.2003.08.024
Siegel H (1997) GIT Fachz Lab 41(5):486–487
Gfrerer M, Stadlober M, Gawlik BM, Wenzl T, Lankmayr E (2001) Chromatographia 53:442–446
Gfrerer M, Serschen M, Lankmayr E (2002) J Biochem Biophys Methods 53:203–216
Gfrerer M, Serschen M, Wenzl T, Gawlik BM, Lankmayr E (2002) Chromatographia 55:467–473
Martens D, Gfrerer M, Wenzl T, Zhang A, Gawlik BM, Schramm K-W, Lankmayr E, Kettrup A (2002) Anal Bioanal Chem 372:562–568; DOI 10.1007/s00216–001–1120-y
Pinhack H (2002) Labor Praxis 6:56–58
Gawlik BM, Platzer B, Muntau H (2000) Monitoring of chlorinated and other organic trace contaminations in selected stretches of the Liao and Yangtse River (China). European Commission EUR 19531 EN, Ispra, Italy
Gawlik BM, Martens D, Henkelmann B, Schramm K-W, Kettrup A, Muntau H (2000) Anal Bioanal Chem 367:232–240
DIN 38414–20 (1996) Deutsche Einheitsverfahren zur Wasser-, Abwasser- und Schlammuntersuchung. Schlamm und Sedimente
Maštovská K, Lehotay SJ (2004) J Chromatogr A 1040:259–272; DOI 10.1016/j.chroma.2004.04.017
Foreman WT, Gates PM (1997) Environ Sci Technol 31:905–910
Acknowledgments.
The series extractor fexIKA Variocontrol was kindly provided by IKA-Labortechnik (Staufen, Germany).
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Gfrerer, M., Fernandes, C. & Lankmayr, E. Optimization of Fluidized-Bed Extraction for Determination of Organochlorine Pesticides in Sediment. Chromatographia 60, 681–686 (2004). https://doi.org/10.1365/s10337-004-0434-2
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1365/s10337-004-0434-2