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Optimization of extractants, purifying packings, and eluents for analytical extraction of organochlorine pesticides in Hydragric Acrisols

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Abstract

In this study, we screened for an economic, rapid, and efficient hypotoxic pretreatment method for organochlorine pesticides in soil samples for gas chromatography (GC) analysis. The analytical extraction efficiencies of 11 different extractants, nine types of solid-phase purification (SPP) cartridge packings, and three types of eluents for 13 organochlorine pesticides (OCPs) in spiked and natural Chinese red soil (Hydragric Acrisols) were evaluated using an ultrasonic extraction and solid-phase purification method. High percent recoveries (85–106%) were obtained for the 13 organochlorine pesticides in soil when petroleum ether/acetone/water (10:5:2, v/v) was used an extractant. They were purified using celite SPP cartridge packing and eluted with 9 mL of dichloromethane/petroleum ether (1:9, v/v). The OCPs purification pretreatment of Hydragric Acrisols, using the above method, meets the GC analysis requirements. Compared with other traditional pretreatment methods for OCPs in soil samples, this method has several advantages, such as a short extraction time, reducing the amount of solvent, having no emulsion phenomenon, and hypotoxicity to the laboratory technicians. The concentrations of 1,1,1,-trichloro-2(p-chlorophenyl)-2-(o-chlorophenyl) ethane (DDTs; 3.42–8.08 ng g−1) in field soils were higher than the hexachlorocyclohexane concentration (2.94–6.12 ng g−1). The 1,1-dichloro-2,2-bis(p-chlorophenyl) ethylene (p,p′-DDE) + 1,1-dichloro-2,2-bis(p-chlorophenyl)-ethane (p,p′-DDD)/p,p'-DDT ratio in this field soil was approximately 2.7, suggesting that no new DDT pollution source was introduced into the sampling site.

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References

  • Anne, M. C., Patricia, A. K., Robert, A. H., & Gerald, T. A. (1996). Extraction and analysis of low concentrations of DDT, DDE and DDD in small volumes of sediment pore water. Chemosphere, 33(7), 1341–1354.

    Article  Google Scholar 

  • Aslam, M. M., Malik, M., Baig, M. A., Qazi, I. A., & Iqbal, J. (2007). Treatment performances of compost-based and gravel-based vertical flow wetlands operated identically for refinery wastewater treatment in Pakistan. Ecological Engineering, 30(1), 34–42.

    Article  Google Scholar 

  • Berdie, L., & Grimalt, J. O. (1998). Assessment of the sample handling procedures in a labor-saving method for the analysis of organochlorine compounds in a large number of fish samples. Journal of Chromatography. A, 823(1–2), 373–380.

    Article  CAS  Google Scholar 

  • Bjorklund, E., von Holst, C., & Anklam, E. (2002). Fast extraction, clean-up and detection methods for the rapid analysis and screening of seven indicator PCBs in food matrices. TrAC Trends in Analytical Chemistry, 21(1), 40–53.

    Article  Google Scholar 

  • Boufatit, M., & Ait-Amar, H. (2007). Removal of N, N-dimethylaniline from a dilute aqueous solution by Na+/K + saturated montmorillonite. Desalination, 206(1–3), 300–310.

    Article  CAS  Google Scholar 

  • Brasquet, C., Bourges, B., & Le Cloirec, P. (1999). Quantitative structure–property relationship (QSPR) for the adsorption of organic compounds onto activated carbon cloth: Comparison between multiple linear regression and neural network. Environmental Science & Technology, 33(23), 4226–4231.

    Article  CAS  Google Scholar 

  • Chen, J., Xia, X., & Ye, X. (2002). Marine organic pollution history in the Changjiang Estuary and Zhejiang coastal area—HCHs and DDTs stratigraphical records. Marine Pollution Bulletin, 45, 391–396.

    Article  CAS  Google Scholar 

  • Chikuni, O., Nhachi, C. F. B., Nyazema, N. Z., Polder, A., Nafstad, I., & Skaare, J. U. (1997). Assessment of environmental pollution by PCBs, DDT and its metabolites using human milk of mothers in Zimbabwe. Science of the Total Environment, 199(1–2), 183–190.

    Article  CAS  Google Scholar 

  • Columé, A., Cárdenas, S., Gallego, M., & Valcarcel, M. (1999). Semiautomatic method for the screening and determination of 23 organochlorine pesticides in horticultural samples by gas chromatography with electron-capture detection. Journal of Chromatography. A, 849(1), 235–243.

    Article  Google Scholar 

  • Concha-Grańa, E., Turnes-Carou, M. I., 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. Journal of Chromatography. A, 1047(1), 147–155.

    Article  Google Scholar 

  • Dabrowska, H., Dabrowski, L., Biziuk, M., Gaca, J., & Namiesnik, J. (2003). Solid-phase extraction clean-up of soil and sediment extracts for the determination of various types of pollutants in a single run. Journal of Chromatography. A, 1003(1–2), 29–42.

    Article  CAS  Google Scholar 

  • Doong, R. A., Peng, C. K., Sun, Y. C., & Liao, P. L. (2002). Composition and distribution of organochlorine pesticide residues in surface sediments from the Wu-Shi River estuary, Taiwan. Marine Pollution Bulletin, 45(1–12), 246–253.

    Article  CAS  Google Scholar 

  • Douglas, E. M., Boakai, K. R., & Martin, A. (2000). Bioavailability to earthworms of aged DDT, DDE, DDD and dieldrin in soil. Environmental Science & Technology, 34(4), 709–713. doi:10.1021/es9909879.

    Article  Google Scholar 

  • FAO/ISRIC/ISSS. (1998). World reference base for soil resources. World soil resources reports (pp. 1–87). Rome: FAO.

    Google Scholar 

  • Flendrig, L. M., Shah, B., Subrahmaniam, N., & Ramakrishnan, V. (2009). Low cost thermoformed solar still water purifier for D&E countries. Physics and Chemistry of the Earth, Parts A/B/C, 34(1–2), 50–54.

    Article  Google Scholar 

  • Folch, I., Vaquero, M. T., Comellas, L., & Broto-Puig, F. (1996). Extraction and clean-up methods for improvement of the chromatographic determination of polychlorinated biphenyls in sewage sludge-amended soils: Elimination of lipids and sulphur. Journal of Chromatography. A, 719(1), 121–130.

    Article  CAS  Google Scholar 

  • Foo, K. Y., & Hameed, B. H. (2010). Detoxification of pesticide waste via activated carbon adsorption process. Journal of Hazardous Materials, 175(1–3), 1–11. doi:10.1016/j.jhazmat.2009.10.014.

    Article  CAS  Google Scholar 

  • Gonzalez, M., Miglioranza, K. S. B., Aizpún de Moreno, J. E., & Moreno, V. J. (2005). Evaluation of conventionally and organically produced vegetables for high lipophilic organochlorine pesticide (OCP) residues. Food and Chemical Toxicology, 43(2), 261–269. doi:10.1016/j.fct.2004.10.002.

    Article  CAS  Google Scholar 

  • Harner, T., Wideman, J. L., & Jantunen, L. M. M. (1999). Residues of organochlorine pesticides in Alabama soils. Environmental Pollution, 106, 323–332.

    Article  CAS  Google Scholar 

  • Hua, X. M., & Shan, Z. J. (1996). The production and application of pesticides and factor analysis of their pollution in environment in China. Advanced Environment Science (China), 2, 33–45. in Chinese.

    Google Scholar 

  • Hussen, A., Westbom, R., Megersa, N., Mathiasson, L., & Bjorklund, E. (2006). Development of a pressurized liquid extraction and clean-up procedure for the determination of α-endosulfan, β-endosulfan and endosulfan sulfate in aged contaminated Ethiopian soils. Journal of Chromatography. A, 1103(2), 202–210.

    Article  CAS  Google Scholar 

  • Jia, Y., Molstad, L., Frostegård, Å., Aagaard, P., Breedveld, G. D., & Bakken, L. R. (2007). Kinetics of microbial growth and degradation of organic substrates in subsoil as affected by an inhibitor, benzotriazole: Model based analyses of experimental results. Soil Biology and Biochemistry, 39(7), 1597–1608.

    Article  CAS  Google Scholar 

  • Jimenez, J. J., Bernal, J. L., Nozal, M. J. D., & Alonso, C. (2004). Liquid–liquid extraction followed by solid-phase extraction for the determination of lipophilic pesticides in beeswax by gas chromatography-electron-capture detection and matrix-matched calibration. Journal of Chromatography. A, 1048(1), 89–97.

    CAS  Google Scholar 

  • Jones, K. C., & de Voogt, P. (1999). Persistent organic pollutants (POPs): State of the science. Environmental Pollution, 100(1–3), 209–221.

    Article  CAS  Google Scholar 

  • Kotowska, U., Garbowska, K., & Isidorov, V. A. (2006). Distribution coefficients of phthalates between absorption fiber and water and its using in quantitative analysis. Analytica Chimica Acta, 560(1–2), 110–117.

    Article  CAS  Google Scholar 

  • Lambropoulou, D. A., Konstantinou, I. K., & Albanis, T. A. (2006). Sample pretreatment method for the determination of polychlorinated biphenyls in bird livers using ultrasonic extraction followed by headspace solid-phase microextraction and gas chromatography–mass spectrometry. Journal of Chromatography. A, 1124(1–2), 97–105.

    Article  CAS  Google Scholar 

  • Lang, Y. H., Cao, Z. M., & Jiang, X. (2005). Prediction of solvents extraction—the organochlorine pesticides in soil using solubility parameter. Talanta, 66(1), 249–252.

    Article  CAS  Google Scholar 

  • Li, J., Zhang, G., Qi, S., Li, X., & Peng, X. (2006). Concentrations, enantiomeric compositions, and sources of HCH, DDT and chlordane in soils from the Pearl River Delta, South China. Science of the Total Environment, 372(1), 215–224.

    Article  CAS  Google Scholar 

  • Ling, Y. C., Teng, H. C., & Cartwright, C. (1999). Supercritical fluid extraction and clean-up of organochlorine pesticides in Chinese herbal medicine. Journal of Chromatography. A, 835(1–2), 145–157.

    Article  CAS  Google Scholar 

  • Lino, C. M., & da Silveira, M. I. N. (1997). Extraction and clean-up methods for the determination of organochlorine pesticide residues in medicinal plants. Journal of Chromatography. A, 769(2), 275–283.

    Article  CAS  Google Scholar 

  • Loganathan, G. B., & Kannan, K. (1994). Global organochlorine contamination trends: An overview. Ambio, 23, 187–190.

    Google Scholar 

  • Manirakiza, P., Covaci, A., Nizigiymana, L., Ntakimazi, G., & Schepens, P. (2002). Persistent chlorinated pesticides and polychlorinated biphenyls in selected fish species from Lake Tanganyika, Burundi, Africa. Environmental Pollution, 117(3), 447–455.

    Article  CAS  Google Scholar 

  • Parera, J., Santos, F. J., & Galceran, M. T. (2004). Microwave-assisted extraction versus Soxhlet extraction for the analysis of short-chain chlorinated alkanes in sediments. Journal of Chromatography. A, 1046(1–2), 19–26.

    CAS  Google Scholar 

  • Prados-Rosales, R. C., Luque Garcia, J. L., & Luque de Castro, M. D. (2003). Rapid analytical method for the determination of pesticide residues in sunflower seeds based on focused microwave-assisted Soxhlet extraction prior to gas chromatography-tandem mass spectrometry. Journal of Chromatography. A, 993(1–2), 121–129.

    Article  CAS  Google Scholar 

  • Qiu, Y., Wen, K., & Bai, H. (1997). Supercritical fluid extraction–gas chromatographic determination of organochlorine pesticide residues in cereals and tea. Chinese Journal of Analytical Chemistry, 25(12), 1391–1394.

    CAS  Google Scholar 

  • Richardson, B. J., & Zheng, G. J. (1999). Chlorinated hydrocarbon contaminants in Hong Kong surficial sediments. Chemosphere, 39(6), 913–923.

    Article  CAS  Google Scholar 

  • Saito, K., Ishizuka, M., & Sugawara, Y. (2004). Cleanup method using disposable tandem cartridge system for the determination of dioxins in human milk by enzyme-linked immunosorbent assay. Bulletin of Environmental Contamination and Toxicology, 73(1), 17–23.

    CAS  Google Scholar 

  • Seidel, V., Tschernuter-Meixner, I., & Lindner, W. (1993). Sandwich-type extraction column with on-line sulphuric acid treatment for the determination of organochlorine compounds in vegetable oil or oil seeds by gas chromatography with electron-capture detection. Journal of Chromatography. A, 642(1–2), 253–262.

    Article  CAS  Google Scholar 

  • Sporring, S., Bowadt, S., Svensmark, B., & Bjorklund, E. (2005). Comprehensive comparison of classic Soxhlet extraction with Soxtec extraction, ultrasonication extraction, supercritical fluid extraction, microwave assisted extraction and accelerated solvent extraction for the determination of polychlorinated biphenyls in soil. Journal of Chromatography. A, 1090(1–2), 1–9.

    Article  CAS  Google Scholar 

  • Tekel, J., & Hatrik, S. (1996). Pesticide residue analyses in plant material by chromatographic methods: Clean-up procedures and selective detectors. Journal of Chromatography. A, 754(1–2), 397–410.

    Article  CAS  Google Scholar 

  • Tor, A., Aydin, M. E., & Özcan, S. (2006). Ultrasonic solvent extraction of organochlorine pesticides from soil. Analytica Chimica Acta, 559(2), 173-180. doi:10.1016/j.aca.2005.11.078.

  • Van Loco, J., Van Leeuwen, S. P. J., Roos, P., Carbonnelle, S., de Boer, J., Goeyens, L., et al. (2004). The international validation of bio- and chemical-analytical screening methods for dioxins and dioxin-like PCBs: The difference project rounds 1 and 2. Talanta, 63(5), 1169–1182.

    Article  Google Scholar 

  • Wei, D., Li, Z., Wang, G., Yang, Y., Li, Y., & Xia, Y. (2006). Separation and purification of natural pyrethrins by reversed phase high performance liquid chromatography. Chinese Journal of Analytical Chemistry, 34(12), 1776–1779.

    Article  Google Scholar 

  • Wiberg, K., Harner, T., Wideman, J. L., & Bidleman, T. F. (2001). Chiral analysis of organochlorine pesticides in Alabama soils. Chemosphere, 45(6–7), 843–848.

    Article  CAS  Google Scholar 

  • Xiong, G., He, X., & Zhang, Z. (2000). Microwave-assisted extraction or saponification combined with microwave-assisted decomposition applied in pretreatment of soil or mussel samples for the determination of polychlorinated biphenyls. Analytica Chimica Acta, 413(1–2), 49–56.

    Article  CAS  Google Scholar 

  • Xu, D., Dan, M., Song, Y., Chai, Z., & Zhuang, G. (2005). Concentration characteristics of extractable organohalogens in PM2.5 and PM10 in Beijing, China. Atmospheric Environment, 39(22), 4119–4128.

    Article  CAS  Google Scholar 

  • Yuan, P., Wu, D., & Weng, W. (2001). Study on surface acid sites of celite and their origins. Acta Mineralogica Sinica, 21(3), 431–434. in Chinese.

    CAS  Google Scholar 

  • Zhou, J. L., Maskaoui, K., Qiu, Y. W., Hong, H. S., & Wang, Z. D. (2001). Polychlorinated biphenyl congeners and organochlorine insecticides in the water column and sediments of Daya Bay, China. Environmental Pollution, 113(3), 373–384.

    Article  CAS  Google Scholar 

  • Zhu, Y., Liu, H., Xi, Z., Cheng, H., & Xu, X. (2005). Organochlorine pesticides (DDTs and HCHs) in soils from the outskirts of Beijing, China. Chemosphere, 60(6), 770–778.

    Article  CAS  Google Scholar 

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Acknowledgments

This work was supported by the National Science and Technology major program (2009ZX07317-007), the National Natural Science Foundation of China (Key Program: 50839002, 21077056), the Ministry of Education Key Laboratory of Integrated Regulation and Resource Development on Shallow Lakes foundation, Hohai University (2007KJ003), and the Fundamental Research Funds for the Central Universities (2009B17014).

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Authors and Affiliations

  1. Key Laboratory for Integrated Regulation and Resources Exploitation on Shallow Lakes, Ministry of Education, Nanjing, 210098, People’s Republic of China

    Zhenhua Zhao

  2. State Key Laboratory of Hydrology-Water Resources and Hydraulic Engineering, Hohai University, Nanjing, 210098, People’s Republic of China

    Zhenhua Zhao

  3. Nanjing Institute of Industry Technology, Nanjing, 210016, People’s Republic of China

    Liling Xia

  4. State Key Laboratory of Soil and Sustainable Agriculture, Institute of Soil Science, Chinese Academy of Sciences, Nanjing, 210008, People’s Republic of China

    Fang Wang & Xin Jiang

  5. College of Resource and Environmental Sciences, Nanjing Agricultural University, Nanjing, 210095, People’s Republic of China

    Yanzheng Gao

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  1. Zhenhua Zhao
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  2. Liling Xia
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  3. Fang Wang
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  4. Xin Jiang
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Correspondence to Zhenhua Zhao or Yanzheng Gao.

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Zhao, Z., Xia, L., Wang, F. et al. Optimization of extractants, purifying packings, and eluents for analytical extraction of organochlorine pesticides in Hydragric Acrisols. Environ Monit Assess 184, 5159–5171 (2012). https://doi.org/10.1007/s10661-011-2330-1

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