Skip to main content

Advertisement

SpringerLink
Log in

Analysis of Organochlorine Pesticides in Coral (Porites evermanni) Samples Using Accelerated Solvent Extraction and Gas Chromatography/Ion Trap Mass Spectrometry

  • Published:
Archives of Environmental Contamination and Toxicology Aims and scope Submit manuscript

Abstract

A gas chromatography/ion trap mass spectrometry method was developed for analysis of organochlorine pesticides (OCPs) in coral samples, which were extracted with accelerated solvent extraction (ASE) and cleaned up on a sulfuric acid-modified silica gel column. The optimal ASE conditions were found to be 100°C and 2000 psi, with a mixture of acetone and methylene chloride (1:1, v/v). The target analytes include hexachlorocyclohexanes (HCHs, specifically, α-, β-, γ-, and δ-HCH isomers), heptachlor, and hexachlorobenzene (HCB), o,p′-, p,p′-dichlorodiphenyltrichloroethane (o,p′-, p,p′-DDT), o,p′-, p,p′-dichlorodiphenyl-dichloroethylene (o,p′-, p,p′-DDE), and o,p′-, p,p′-dichlorodiphenyldichloroethane (o,p′-, p,p′-DDD). Standard sand samples were used as an alternative matrix spiked with OCP standards to determine the method precision and accuracy. Average recoveries of OCPs ranged from 82% to 102%, with relative standard deviations (RSDs) of 3%–6%, at a level of 10 ng/g and from 50% to 68%, with RSDs of 13%–19% at a level of 2 ng/g. The developed method was applied for analysis of OCPs in coral samples collected from Tern Island and Bikini Atoll in the Pacific Ocean. The concentrations of HCB were 7–26 pg/g dry weight in the samples from Bikini Atoll and 3–45 pg/g in those from Tern Island, and heptachlor concentrations were 208–2200 and 44–104 pg/g in the coral samples from Bikini Atoll and Tern Island, respectively. ∑HCH (sum of α-, β-, γ-, and δ-HCH) were 8–82 pg/g in Bikini Atoll coral and 86–629 pg/g in Tern island coral, and ∑DDT (sum of o,p′-, p,p′-DDD, o,p′-, p,p′-DDE, and o,p′- p,p′-DDT) were 80–212 pg/g in Bikini Atoll coral and 593–3165 pg/g in Tern Island coral. The results suggest that coral is a viable indicator species for pollution monitoring, which pollutants and their concentrations may be related to dated carbonate layers.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3

Similar content being viewed by others

References

  • Ahmad UK, Ujang Z, Woon CH, Indran S, Mian MN (2004) Development of extraction procedures for the analysis of polycyclic aromatic hydrocarbons and organochlorine pesticides in municipal sewage sludge. Water Sci Technol 50:137–144

    CAS  Google Scholar 

  • Ahmed E (2003) Analysis of polychlorinated biphenyls in food products. Trends Anal Chem 22:170–185

    Article  CAS  Google Scholar 

  • Björklund E, Nilsson T, Bøwadt S (2000) Pressurised liquid extraction of persistent organic pollutants in environmental analysis. Trends Anal Chem 19:434–445

    Article  Google Scholar 

  • Concha-Grana E, Turnes-Carou MI, Muniategui-Lorenzo S, Lopez-Mahia P, Fernandez-Fernandez E, Prada-Rodriguez D (2004) Development of pressurized liquid extraction and cleanup procedures for determination of organochlorine pesticides in soils. J Chromatogr A 1047:147–155

    Article  CAS  Google Scholar 

  • Delgado JP (1996) Ghost fleet, the sunken ships of Bikini Atoll. University of Hawaii Press, Honolulu, p 204

    Google Scholar 

  • Eljarrat E, Barceló D (2004) Sample handling and analysis of brominated flame retardants in soil and sludge samples. Trends Anal Chem 23:727–736

    Article  CAS  Google Scholar 

  • El Nemr A, El-Sikaily A, Khaled A, Said TO, Abd-Allah AMA (2004) Chlorinated pesticides and polychlorinated biphenyls in the coral reef skeleton of the Egyptian Red Sea Coast. Bull Environ Contam Toxicol 72:1195–1202

    Article  CAS  Google Scholar 

  • El-Sikaily A, Khaled A, EI Nemr A, Said TO, Abd-Alla AMA (2003) Polycyclic aromatic hydrocarbons and aliphatics in the coral reef skeleton of the Egyptian Red Sea Coast. Bull Environ Contam Toxicol 71:1252–1259

    Article  CAS  Google Scholar 

  • Fatoki OS, Awofolu RO (2003) Methods for selective determination of persistent organochlorine pesticide residues in water and sediments by capillary gas chromatography and electron-capture detection. J Chromatogr A 983:225–236

    Article  CAS  Google Scholar 

  • Fisher JA, Scarlett MJ, Stott AD (1997) Accelerated solvent extraction: an evaluation for screening of soils for selected U.S. EPA semivolatile organic priority pollutants. Environ Sci Technol 31:1120–1127

    Article  CAS  Google Scholar 

  • Frenich AG, Vidal JL, Frias MM, Olea-Serrano F, Olea N (2000). Quantitative determination of endocrine-disrupting polychlorinated biphenyls and organochlorinated pesticides in human serum using gas chromatography with electron-capture detection and tandem mass spectrometry. J Mass Spectrom 35:967–975

    Article  CAS  Google Scholar 

  • Gan J, Papiernik SK, Koskinen WC, Yates SR (1999) Evaluation of accelerated solvent extraction (ASE) for analysis of pesticide residues in soil. Environ Sci Technol 33:3249–3253

    Article  CAS  Google Scholar 

  • Glynn PW, Howard LS, Corcoran E, Freay AD (1984) The occurrence and toxicity of herbicides in reef building corals. Mar Pollut Bull 15:370–374

    Article  CAS  Google Scholar 

  • Hatcher BG, Johannes RE, Robertson AI (1989) Review of research relevant to the conservation of shallow tropical marine ecosystems. Ocean Mar Bio Annu Rev 27:337–414

    Google Scholar 

  • Hawthorne SB, Grabanski CB, Martin E, Miller DJ (2000) Comparisons of Soxhlet extraction, pressurized liquid extraction, supercritical fluid extraction and subcritical water extraction for environmental solids: recovery, selectivity and effects on sample matrix. J Chromatogr A 892:421–433

    Article  CAS  Google Scholar 

  • Heemken OP, Theobald N, Wenclawiak BW (1997) Comparison of ASE and SFE with Soxhlet, sonication, and methanolic saponification extractions for the determination of organic micropollutants in marine particulate matter. Anal Chem 69:2171–2180

    Article  CAS  Google Scholar 

  • Hughes TP (1994) Catastrophes, phase shifts and large scale degradation of a Carribbean coral reef. Science 265:1547–1551

    Article  Google Scholar 

  • Khaled A, EI Nemr A, EI Sikaily A (2003) Contamination of coral reef by heavy metals along the Egyptian Red Sea coast. Bull Environ Contam Toxicol 71:577–584

    Article  CAS  Google Scholar 

  • Lopez-Avila V, Bauer K, Milanes J, Beckert WF (1993) Evaluation of soxtec extraction procedure for extracting organic compounds from soils and sediments. J AOAC Int 76:864–880

    CAS  Google Scholar 

  • Loya Y, Rinkevich B (1980) Effects of oil pollution on coral reef communities. Mar Ecol Prog Ser 3:167–180

    Article  Google Scholar 

  • Martens D, Gferer M, Wenzl T, Zhang A, Gawlik BM, Schramm KW (2002) Comparison of different extraction techniques for the determination of polychlorinated organic compounds in sediment. Anal Bioanal Chem 372:562–568

    Article  CAS  Google Scholar 

  • Meehan W, Ostrander GK (1997) Coral bleaching: a potential biomarker of environmental stress. J Toxicol Environ Health 50:529–552

    Article  CAS  Google Scholar 

  • Miao XS, Swenson C, Woodward L, Li QX (2000a) Distribution of polychlorinated biphenyls in marine species from French Frigate Shoals, North Pacific Ocean. Sci Total Environ 257:17–28

    Article  CAS  Google Scholar 

  • Miao XS, Swenson C, Yanagihara K, Li QX (2000b) Polychlorinated biphenyls and metals in marine species from French Frigate Shoals, North Pacific Ocean. Arch Environ Contam Toxicol 38: 464–471

    Article  CAS  Google Scholar 

  • Raloff J (1999) Sea sickness, marine epidemiology comes of age. Sci News 155:72–74

    Article  Google Scholar 

  • Rogers CS (1989) Responses of coral reefs and reef organisms to sedimentation. Mar Ecol Prog Ser 62:185–202

    Article  Google Scholar 

  • Pastorok RA, Bilyard GR (1985) Effect of sewage pollution on coral-reef communities. Mar Ecol Prog Ser 21:175–189

    Article  Google Scholar 

  • Patel K, Fussell RJ, Hetmanski M, Goodall DM, Keely BJ (2005) Evaluation of gas chromatography–tandem quadrupole mass spectrometry for the determination of organochlorine pesticides in fats and oils. J Chromatogr A 1068:289–296

    Article  CAS  Google Scholar 

  • Peters EC (1984) A survey of cellar reactions to environmental stress and disease in Caribbean scheractinian corals. Helgoländer Meeresunter 37:113–137

    Article  Google Scholar 

  • Phillips DJH, Tanabe S (1989) Aquatic pollution in the Far East. Mar Pollut Bull 20:297–303

    Article  CAS  Google Scholar 

  • Popp P, Keil P, Moëeder M, Paschke A, Thuss U (1997) Application of accelerated solvent extraction followed by gas chromatography, high-performance liquid chromatography and gas chromatography–mass spectrometry for the determination of polycyclic aromatic hydrocarbons, chlorinated pesticides and polychlorinated dibenzo-p-dioxins and dibenzofurans in solid wastes. J Chromatogr A 774:203–211

    Article  Google Scholar 

  • Pyle SM, Marcus ABJ (1997) Rapid and sensitive determination of pesticides in environmental samples by accelerated solvent extraction and tandem mass spectrometry. J Mass Spectrom 32:897–898

    Article  CAS  Google Scholar 

  • Richter BE, Jones BA, Ezzell JL, Porter NL, Avdalovic N, Pohl C (1996) Accelerated solvent extraction: a technique for sample preparation. Anal Chem 68:1033–1039

    Article  CAS  Google Scholar 

  • Richter BE, Ezzell JL, Knowles DE, Hoefler F, Mattulat AKR, Scheutwinkel M, Waddell DS, Gobran T, Khurana V (1997) Extraction of polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans from environmental samples using accelerated solvent extraction (ASE). Chemosphere 34:975–987

    Article  CAS  Google Scholar 

  • Saim N, Dean JR, Abdullah P, Zakaria Z (1998) An experimental design approach for the determination of polycyclic aromatic hydrocarbons from highly contaminated soil using accelerated solvent extraction. Anal Chem 70:420–424

    Article  CAS  Google Scholar 

  • Sannino A, Mambriani P, Bandini M, Bolzoni L (1996) Multiresidue method for determination of organochlorine insecticides and polychlorinated biphenyl congeners in fatty processed foods. J AOAC Int 79:1434–1446

    CAS  Google Scholar 

  • Schantz MM, Nichols JJ, Wise SA (1997) Evaluation of pressurized fluid extraction for the extraction of environmental matrix reference materials. Anal Chem 69:4210–4219

    Article  CAS  Google Scholar 

  • Serrano R, Barreda M, Pitarch E, Hernández F (2003) Determination of low concentrations of organochlorine pesticides and PCBs in fish feed and fish tissues from aquaculture activities by gas chromatography with tandem mass spectrometry. J Sep Sci 26:75–86

    Article  CAS  Google Scholar 

  • Sterzenbach D, Wenclawiak BW, Weigelt V (1997) Determination of chlorinated hydrocarbons in marine sediments at the part-per-trillion level with supercritical fluid extraction. Anal Chem 69:831–836

    Article  CAS  Google Scholar 

  • Tanabe S, Senthikumar K, Kannan K, Subramanian AN (1998) Accumulation features of polychlorinated biphenyls and organochlorine pesticides in resident and migratory birds from South India. Environ Contam Toxicol 34:387–397

    Article  CAS  Google Scholar 

  • Thompson S, Budzinski H, Garriguse P, Narbonne F (1999) Comparison of PCB and DDT distribution between water-column and sediment-dwelling bivalves in Arcachon Bay, France. Mar Pollut Bull 38:655–662

    Article  CAS  Google Scholar 

  • Thompson S, Budzinski H, LeMenach K, Letellier M, Garriges P (2002) Multi-residue analysis of polycyclic aromatic hydrocarbons, polychlorobiphenyls, and organochlorine pesticides in marine sediments. Anal Bioanal Chem 372:196–204

    Article  CAS  Google Scholar 

  • U.S. EPA (1998) Pressurized fliud extraction (PFE). Method 3545A. U.S. EPA, Washington, DC

  • Vetter W, Weichbrodt M, Scholz E, Luckas B, Oelschlager H (1999) Levels of organochlorines (DDT, PCBs, Toxaphene, Chlordane, Dieldrin, and HCHs) in blubber of South African Fur Seals (Arctocephalus pusillus pusillus) from Cape Cross/ Namibia. Mar Pollut Bull 38:830–836

    Article  CAS  Google Scholar 

  • Wang D, Atkinson S, Hoover-Miller A, Li QX (2005) Analysis of organochlorines in harbor seal (Phoca vitulina) tissue samples from Alaska using gas chromatography/ion trap mass spectrometry by an isotopic dilution technique. Rapid Commun Mass Spectrom 19:1815–1821

    Article  CAS  Google Scholar 

  • Wenzel KD, Hubert A, Manz M, Weissflog L, Engewald W, Schrann G (1998) Accelerated solvent extraction of semivolatile organic compounds from biomonitoring samples of pine needles and mosses. Anal Chem 70:4827–4835

    Article  CAS  Google Scholar 

Download references

Acknowledgments

This work was funded, partly, by the U.S. Fish and Wildlife Service and Hawaii Heptachlor Research & Education Foundation (HHHERP 98–05). We would like to acknowledge U. Hans Beiling of S. Cohen & Associates for providing the coral samples collected from Bikini Atoll, Republic of the Marshall Islands.

Author information

Author notes

  1. Xiusheng Miao

    Present address: ArQule, Inc., Woburn, MA, 01801, USA

Authors and Affiliations

  1. Department of Molecular Biosciences and Bioengineering, University of Hawaii at Manoa, Honolulu, Hawaii, 96822, USA

    Dongli Wang, Xiusheng Miao & Qing X. Li

Authors
  1. Dongli Wang
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Xiusheng Miao
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Qing X. Li
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Qing X. Li.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Wang, D., Miao, X. & Li, Q.X. Analysis of Organochlorine Pesticides in Coral (Porites evermanni) Samples Using Accelerated Solvent Extraction and Gas Chromatography/Ion Trap Mass Spectrometry. Arch Environ Contam Toxicol 54, 211–218 (2008). https://doi.org/10.1007/s00244-007-9016-2

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s00244-007-9016-2

Keywords

Search

Navigation