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An expeditious method for the determination of organochlorine pesticides residues in estuarine sediments using microwave assisted pre-extraction and automated headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry.
Talanta. 2008 Sep 15; 76(5):1124-9.T

Abstract

Determination of organochlorine pesticides (OCPs) in sediments implicates extraction of these compounds from the matrix, which is difficult owing to strong interaction among OCPs and different constituents of the sediments, particularly organic content. The method here described is a combination of microwave assisted extraction (MAE), headspace solid-phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS), acting in selected-ion storage mode, or GC-electron capture detector (ECD, for routine analysis). Methanol was used as extracting solvent and aliquots of the MAE extracts (after inclusion of a step for sulfur elimination when required) were used to prepare aqueous solutions for HS-SPME. A complete automation of the SPME procedure increases the sample throughput, including standard addition for calibration purpose. The procedure has the advantage of exclude additional clean-up steps and pre-concentration before SPME. Application to reference sediments of different characteristics revealed absence of significant interferences from the matrix for alpha-lindane, gamma-lindane, aldrin, dieldrin, endrin, 4,4'-DDT, 4,4'-DDD, 4,4'-DDE, heptachlor, heptachlor epoxide and good sensitivity. Detection limits ranged from 0.005 to 0.11 ng of OCP per gram of dried sediment using GC-MS and from 0.01 to 0.26 ngg(-1) using GC-ECD. The linear response ranges embraced 5-6 orders of magnitude (up to 1000 ngg(-1)) in GC-MS, being narrower for GC-ECD. The method was successfully applied to sandy and muddy sediments from Portuguese rivers estuaries, enabling quantification of seven OCPs. The method resulted effective, relatively simple and fast, being suitable for routine monitoring of residues of OCPs from sediments of different grain size and organic matter content, which influence concentration, mobility and availability of contaminants.

Authors+Show Affiliations

CIMAR/CIIMAR - Centro Interdisciplinar de Investigação Marinha e Ambiental and Faculdade de Ciências, Universidade do Porto, R. Campo Alegre 687, Porto 4169-007, Portugal.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

18761165

Citation

Carvalho, Pedro N., et al. "An Expeditious Method for the Determination of Organochlorine Pesticides Residues in Estuarine Sediments Using Microwave Assisted Pre-extraction and Automated Headspace Solid-phase Microextraction Coupled to Gas Chromatography-mass Spectrometry." Talanta, vol. 76, no. 5, 2008, pp. 1124-9.
Carvalho PN, Rodrigues PN, Alves F, et al. An expeditious method for the determination of organochlorine pesticides residues in estuarine sediments using microwave assisted pre-extraction and automated headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry. Talanta. 2008;76(5):1124-9.
Carvalho, P. N., Rodrigues, P. N., Alves, F., Evangelista, R., Basto, M. C., & Vasconcelos, M. T. (2008). An expeditious method for the determination of organochlorine pesticides residues in estuarine sediments using microwave assisted pre-extraction and automated headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry. Talanta, 76(5), 1124-9. https://doi.org/10.1016/j.talanta.2008.05.035
Carvalho PN, et al. An Expeditious Method for the Determination of Organochlorine Pesticides Residues in Estuarine Sediments Using Microwave Assisted Pre-extraction and Automated Headspace Solid-phase Microextraction Coupled to Gas Chromatography-mass Spectrometry. Talanta. 2008 Sep 15;76(5):1124-9. PubMed PMID: 18761165.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - An expeditious method for the determination of organochlorine pesticides residues in estuarine sediments using microwave assisted pre-extraction and automated headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry. AU - Carvalho,Pedro N, AU - Rodrigues,Pedro Nuno R, AU - Alves,Filipe, AU - Evangelista,Rafael, AU - Basto,Maria Clara P, AU - Vasconcelos,M Teresa S D, Y1 - 2008/07/07/ PY - 2008/01/17/received PY - 2008/05/09/revised PY - 2008/05/14/accepted PY - 2008/9/2/pubmed PY - 2008/10/31/medline PY - 2008/9/2/entrez SP - 1124 EP - 9 JF - Talanta JO - Talanta VL - 76 IS - 5 N2 - Determination of organochlorine pesticides (OCPs) in sediments implicates extraction of these compounds from the matrix, which is difficult owing to strong interaction among OCPs and different constituents of the sediments, particularly organic content. The method here described is a combination of microwave assisted extraction (MAE), headspace solid-phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS), acting in selected-ion storage mode, or GC-electron capture detector (ECD, for routine analysis). Methanol was used as extracting solvent and aliquots of the MAE extracts (after inclusion of a step for sulfur elimination when required) were used to prepare aqueous solutions for HS-SPME. A complete automation of the SPME procedure increases the sample throughput, including standard addition for calibration purpose. The procedure has the advantage of exclude additional clean-up steps and pre-concentration before SPME. Application to reference sediments of different characteristics revealed absence of significant interferences from the matrix for alpha-lindane, gamma-lindane, aldrin, dieldrin, endrin, 4,4'-DDT, 4,4'-DDD, 4,4'-DDE, heptachlor, heptachlor epoxide and good sensitivity. Detection limits ranged from 0.005 to 0.11 ng of OCP per gram of dried sediment using GC-MS and from 0.01 to 0.26 ngg(-1) using GC-ECD. The linear response ranges embraced 5-6 orders of magnitude (up to 1000 ngg(-1)) in GC-MS, being narrower for GC-ECD. The method was successfully applied to sandy and muddy sediments from Portuguese rivers estuaries, enabling quantification of seven OCPs. The method resulted effective, relatively simple and fast, being suitable for routine monitoring of residues of OCPs from sediments of different grain size and organic matter content, which influence concentration, mobility and availability of contaminants. SN - 1873-3573 UR - https://www.unboundmedicine.com/medline/citation/18761165/An_expeditious_method_for_the_determination_of_organochlorine_pesticides_residues_in_estuarine_sediments_using_microwave_assisted_pre_extraction_and_automated_headspace_solid_phase_microextraction_coupled_to_gas_chromatography_mass_spectrometry_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0039-9140(08)00397-4 DB - PRIME DP - Unbound Medicine ER -