Determination of OCPs and PCBs in environmental water samples by GC-DLLME optimized by Response Surface Methodology

  • Dekun Hou College of Ecology and Environment of Inner Mongolia University, Hohhot, 010021, China
  • Otgonbayar Khureldavaa Institute of Chemistry and Chemical Technology, Mongolian Academy of Sciences, 4th Bulding of MAS, Ulaanbaatar, 13330, Mongolia
  • Fujin Zhang Institute of Environmental Resources and Analytical Technique, Inner Mongolia Academy of Agricultural and Animal Husbandry Sciences, Hohhot, 010031, China
  • Jiang He College of Ecology and Environment of Inner Mongolia University, Hohhot, 010021, China
  • Badgaa Amarsanaa Institute of Chemistry and Chemical Technology, Mongolian Academy of Sciences, 4th Building of MAS, Ulaanbaatar, 13330, Mongolia
Keywords: Organochlorine pesticides, dispersive liquid-liquid microextraction, environmental waters, response surface methodology, polychlorinated biphenyls


A new sample preparation procedure to determine seven organochlorine pesticides and seven polychlorinated biphenyls in environmental water samples by using a combination of ultrasonic-assisted solvent extraction and dispersive liquid-liquid micro-extraction was established, and the extracted analytes were analyzed by gas chromatography coupled with electron capture detector. Some parameters influencing the extraction efficiency were studied and optimized utilizing response surface methodology. Under the optimum extraction conditions, the method showed wide linear ranges with r2 > 0.9989 and low limits of detection and quantification between 0.16 ~ 2.17 μg/L and 0.53 ~ 7.16 μg/L, respectively. Enrichment factors (EF) were high and ranged from 63 to 116. Relative standard deviations (RSDs) for the extraction of 25 μg/L of each selected OCPs and PCBs were less than 10.2 %. The proposed method was successfully used for targets contaminations determination in different water samples. α-HCH, β-HCH and p,p’-DDE were found in lake water closed to farmland with concentrations of 2.56 μg/L, 4.44 μg/L and 4.74 μg/L, respectively, and other OCPs and PCBs were not found in the corresponding water samples. The relative recoveries of OCPs and PCBs from tap water, river water and lake water at spiking levels of 10 μg/L were in the range of 81.9 ~ 109.7 %, within a relative standard deviation of 1.7 ~ 11.8 %. The results revealed that the proposed method was well suited for the determination of trace amounts of target contaminations in liquid samples.


Author Biography

Dekun Hou, College of Ecology and Environment of Inner Mongolia University, Hohhot, 010021, China

Weihai Institutes of Supervision & Inspection for Products Quality, Weihai, 264209, China


Alonso-Hernandez C.M., Mesa-Albernas M., Tolosa I. (2014) Organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) in sediments from the Gulf of Batabano, Cuba. Chemosphere, 94, 36-41.

Shao Y., Han S., Ouyang J., Yang G.S., Liu W.H., (2016) Organochlorine pesticides and polychlorinated biphenyls in surface water around Beijing. Environ. Sci. Pollut. Res., 23(24), 24824-24833.

Combi T., Taniguchi S., Figueira R.C., Mahiques M.M., Martins C.C. (2013) Spatial distribution and historical input of polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs) in sediments from a subtropical estuary (Guaratuba Bay, SW Atlatic).Mar. Pollut. Bull., 70(1-2), 247-252.

Roszko M., Jędrzejczak R., Szymczyk K. (2014) Polychlorinated biphenyls (PCBs), polychlorinated diphenyls ethers (PBDEs) and organochlorine pesticides in selected cereals available on the Polish retail market. Sci. Total. Environ., 466-467, 136-151.

Klil-Drori A.J., Kleinstern G., Seir R.A., Choshen-Cohen L., Abdeen Z. (2018) Serum organochlorines and non-Hodgkin lymphoma: A case-control study in Israeli Jews and Palestinians. Chemosphere, 213, 395-402.

Li Y., Chen P., Huang S. (2013) Water with low concentration of surfactant in dispersed solvent-assisted emulsion dispersive liquid-liquid microextraction for the determination of organochlorine pesticides in aqueous samples. J. Chromatography A, 1300, 51-57.

Kim M., Song N.R., Hong J.K., Lee J., Pyo H. (2013) Quantitative analysis of organochlorine pesticides in human serum using headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry. Chemosphere, 92, 279-285.

Zhou Q., Wang J.J., Meng B.D., Cheng J.Q., Lin G.P (2013) Distribution and sources of organochlorine pesticides in agricultural soils from central China. Ecotox. Environ. Safe., 93, 163-170.

Ouyang H.L., Wang Q.M., He W., Qin N., Kong X.Z (2014) Organochlorine pesticides in the dust fall around Lake Chaohu, the fifth largest lake in China. Environ. Monit. Assess., 186, 383-393.

Stockholm Convention. 2009.

Martins J.G., Chávez A.A., Waliszewski S.M., Cruz A.C. (2013) Extraction and clean-up methods for organochlorine pesticides determination in milk. Chemosphere, 92, 233-246.

Fu J.M., Mai B.X., Sheng G.Y., Zhang G., Wang X.M. (2003) Persistent organic pollutants in environment of the Pearl river Delta, China: An Overview. Chemosphere, 52, 1411-1422.

Shi Y.J., Lu Y.L., Meng F.Q., Guo F.F., Zheng X.Q. (2013) Occurrence of organic chlorinated pesticides and their ecological effects on soil protozoa in the agricultural soils of North Western Beijing, China. Ecotoxicol. Environ. Safe., 92, 123-128.

Yuan L.X., Qi S.H., Wu X.G., Wu C.X., Xing X.L (2013) Spatial and temporal variations of organochlorine pesticides (OCPs) in water and sediments from Honghu Lake, China. J. Geochem. Explor., 132, 181-187.

Harrad S., Goosey E., Desborough J., Abdallah M.A., Roosens L (2010) Dust from U.K. primary school classrooms and daycare centers: the significance of dust as a pathway of exposure of young U.K. children to brominated flame retardants and polychlorinated biphenyls. Environ. Sci. Technol., 44, 4198-4202.

Lin W., Jiang R.F., Xiong Y.X., Wu J.Y., Xu J.Q (2019) Quantification of the combined toxic effect of polychlorinated biphenyls and nano-sized polystyrene on Daphnia magna. J. Hazard. Mater., 364, 531-536.

Perugini M., Manera M., Tavoloni T., Lestingi C., Pecorelli I (2013) Temporal trends of PCBs in feed and dietary influence in farmed rainbow trout (Oncorhynchus mykiss). Food Chem., 141(3), 2321-2327.

Baert J.M., Janssen C.R., Borga K., De Laender F. (2013) Migration and opportunistic feeding increase PCB accumulation in Arctic seabirds. Environ. Sci. Technol., 47(20), 11793-11801.

Rosenfelder N., Vetter W. (2014) Polychlorinated terphenyl patterns and levels in selected marine mammals and a river fish from different continents. Environ. Inter., 62, 119-124.

Navarro-Ortega A., Tauler R., Lacorte S., Barcelo D. (2010) Occurrence and transport of PAHs, pesticides and alkylphenols in sediment samples along the Ebro River Basin. J. Hydrol., 383(1), 5-17.

Zhang Y.Z., Tang C.Y., Song X.F., Dun Y., Meng W (2013) Concentrations, potential sources and behavior of organochlorines and phenolic endocrine-disrupting chemicals in surficial sediment of the Shaying River, eastern China. Environ. Earth. Sci., 70(5), 2237-2247.

Sibali L.L., Okwonkwo J.O., McCrindle R.I. (2008) Determination of selected organochlorine pesticide (OCP) compounds from the Jukskei River catchment area in Gauteng, South Africa. Water SA, 34(5), 611-622.

Ta N., Zhou F., Gao Z.Q., Zhong M., Sun C. (2006) The status of pesticide residues in the drinking water sources in Meiliangwan Bay, Taihu lake of China. Environ. Monit. Assess., 123(1-3), 351-370.

Gao L.L., Yan C.H., Yu X.D., Tian Y., Zou X.Y (2012) Determination of polychlorinated biphenyls and organochlorine pesticides in human serum by gas chromatography with micro-electron capture detector. J. Chroma. Sci., 50(2), 145-150.

Popp P., Bauer C., Mӧder M., Paschke A. (2000) Determination of polycyclic aromatic hydrocarbons in waste water by off-line coupling of solid-phase microextraction with column liquid chromatography. J. Chromatography A, 897(1-2), 153-159.

Stack M.A., Fitzgerald G., O'Connell S., James K.J. (2000) Measurement of trihalomethanes in potable and recreational waters using solid phase micro extraction with gas chromatography-mass spectrometry. Chemosphere, 41(11), 1821-1826.

Cho D.H., Kong S.H., Oh S.G. (2003) Analysis of trihalomethanes in drinking water using headspace-SPME technique with gas chromatography. Water Res., 37(2), 402-408.

Shen G., Lee H.K. (2002) Hollow fiber-protected liquid-phase microextraction of triazine herbicides. Anal. Chem., 74(3), 648-654

Ahmadi F., Assadi Y., Milani Hosseini S.M.R., Rezaee M. (2006) Determination of organophosphorus pesticides in water samples by single drop microextraction and gas chromatography-flame photometric detector. J. Chromatography A, 1101(1-2), 307-312.

Rezaee M., Assadi Y., Milani Hosseini S.M.R., Aghaee E., Ahmadi F (2006) Determination of organic compounds in water using dispersive liquid-liquid microextraction. J. Chromatography A, 1116 (1), 1-9.

Zhao X., Fu L., Hu J., Li J., Wang H (2009) Analysis of PAHs in water and fruit juice samples by DLLME combined with LC-Fluorescence detection. Chromatographia, 69(11), 1-5.

Meryemoglu B., Hasanoglu A., Kaya B., Irmak S., Erbatur O. (2014) Hydrogen production from aqueous-phase reforming of sorghum biomass: An application of the response surface methodology. Renewable Energy, 62, 535-541.

Zhang Y.B., Wang L.H., Zhang D.Y., Zhou L.L., Guo Y.X. (2014) Ultrasound-assisted extraction and purification of schisandrin B from Schisandra chinensis (Turcz) Baill seeds: optimization by response durface methodology. Ultrason. Sonochem., 21(2), 461-466.

How to Cite
Hou, D., Khureldavaa, O., Zhang, F., He, J., & Amarsanaa, B. (2019). Determination of OCPs and PCBs in environmental water samples by GC-DLLME optimized by Response Surface Methodology. Mongolian Journal of Chemistry, 20(46), 13-23.