Citation: Li Zhang, Guang-Shui Na, Chun-Xiang He, Rui-Jing Li, Hui Gao, Lin-Ke Ge, Yan-Jie Wang, Yao Yao. A novel method through solid phase extraction combined with gradient elution for concentration and separation of 66 (ultra) trace persistent toxic pollutants in Antarctic waters[J]. Chinese Chemical Letters, ;2016, 27(03): 405-411. doi: 10.1016/j.cclet.2015.12.001 shu

A novel method through solid phase extraction combined with gradient elution for concentration and separation of 66 (ultra) trace persistent toxic pollutants in Antarctic waters

Li Zhang ^a,b ,
Guang-Shui Na ^b,, ,
Chun-Xiang He ^a,, ,
Rui-Jing Li ^b ,
Hui Gao ^b ,
Lin-Ke Ge ^b ,
Yan-Jie Wang ^b ,
Yao Yao ^b

a.
a. School of Chemistry and Chemical Engineering, Liaoning Normal University, Dalian 116029, China;
b.
b. Key Laboratory for Ecological Environment in Coastal Areas (SOA), National Marine Environmental Monitoring Center, Dalian 116023, China

Corresponding author: Guang-Shui Na, Chun-Xiang He,
Received Date: 6 September 2015
Available Online: 4 November 2015
Fund Project: This work was financially supported by the National Natural Science Foundation of China (No.21377032) (No.21377032) the Marine Public Welfare Scientific Research Projects (No.201105013) (Nos.2014-02-01, 2014-03-04, 2014-04-01, 2014-04-03)the Foundation of Polar Science Key Laboratory, SOA, China (No.KP201208). (No.201105013)

This study developed a method to perform the simultaneous concentration and selective separation of 66 (ultra) trace persistent toxic substances in Antarctic waters. The substances included 30 polychlorinated biphenyls, 17 organochlorine pesticides, 16 polycyclic aromatic hydrocarbons, 3 hexabromocyclododecanes. Solid phase extraction was performed using a C₁₈ membrane and silica gel column. Gradient elution was conducted using organic solvents with different polarities; as a result, the efficiency of the C₁₈ film is improved and the interferences from impurities and target compounds are eliminated. Extracts were subsequently analyzed through gas chromatography or liquid and gas chromatography coupled to tandem mass spectrometry. Method validation yielded the following values:recoveries of all target analytes in the Antarctic water ranged from 87.3% to 117.6% and reproducibility as percent relative standard deviation was lower than 5%. Quantification limits ranged from 0.004 μg L^-1 to 0.030 μg L^-1. The established method improved the recoveries and reduced the limits of detection. Results indicated the method exhibited good performance in the simultaneous concentration and selective separation of 66 (ultra) trace organic pollutants; Therefore, the proposed sample pretreatment can potentially eliminate the effects of various classes of impurities to some extent.
1. [1]
  [1] M.A.E. Abdallah, D. Drage, S. Harrad, A one-step extraction/clean-up method for determination of PCBs, PBDEs and HBCDs in environmental solid matrices, Environ. Sci. Pro. (Ⅰ)mpacts 15(2013) 2279-2287.
2. [2]
  [2] L. Wolska, Miniaturised analytical procedure of determining polycyclic aromatic hydrocarbons and polychlorinated biphenyls in bottom sediments, J. Chromatogr. A 959(2002) 173-180.
3. [3]
  [3] A. Mahmood, R.N. Malik, J. Li, G. Zhang, Levels, distribution pattern and ecological risk assessment of organochlorines pesticides (OCPs) in water and sediments from two tributaries of the Chenab River, Pakistan, Ecotoxicology 23(2014) 1713-1721.
4. [4]
  [4] R. Sarria-Villa,W. Ocampo-Duque, M. Páez, M. Schuhmacher, Presence of PAHs in water and sediments of the Colombian Cauca River during heavy rain episodes, and implications for risk assessment, Sci. Total Environ. (2015), doi:10.1016.
5. [5]
  [5] M.(Ⅰ).H. Helaleh, A. Al-Rashdan, A. (Ⅰ)btisam, Simultaneous analysis of organochlorinated pesticides (OCPs) and polychlorinated biphenyls (PCBs) from marine samples using automated pressurized liquid extraction (PLE) and Power PrepTM clean-up, Talanta 94(2012) 44-49.
6. [6]
  [6] G.B. Kim, H.M. Stapleton, PBDEs, methoxylated PBDEs and HBCDs in Japanese common squid (Todarodes pacificus) from Korean offshore waters, Mar. Pollut. Bull. 60(2010) 935-940.
7. [7]
  [7] G.L. Mihalca, O. Tiţa, M. Tiţa, A. Mihalca, Polycyclic aromatic hydrocarbons (PAHs) in smoked fish from three smoke-houses in Braşov County, J. Agroaliment. Proc. Technol. 17(2011) 392-397.
8. [8]
  [8] M.H. Son, J. Kim, E.S. Shin, S.H. Seo, Y.S. Chang, Diastereoisomer-and speciesspecific distribution of hexabromocyclododecane (HBCD) in fish and marine invertebrates, J. Hazard. Mater. 300(2015) 114-120.
9. [9]
  [9] Y.M. Sun, Y.F. Wang, F. Liu, et al., Determining semi-volatile organic substances of groundwater through liquid-liquid extraction-C₁₈ membrane disk extraction-GS/MS, J. Chin. Mass. Spectr. Soc. 27(2006) 140-147.
10. [10]
  [10] B.H. Jin, F. Xiao, B. Chen, P.J. Chen, L.Q. Xie, Determination of 27 poison compounds in bottled drinking water by combining C₁₈ solid-phase membrane extraction with GC-MS technique, Chin. J. Anal. Lab. 28(2009) 99-102.
11. [11]
  [11] T. Trtić-Petrović, J. Dordević, N. Dujaković, et al., Determination of selected pesticides in environmental water by employing liquid-phase microextraction and liquid chromatography-tandem mass spectrometry, Anal. Bioanal. Chem. 397(2010) 2233-2243.
12. [12]
  [12] N. Dujaković, S. Grujić, M. Radišić, T. Vasiljević, M. Laušević, Determination of pesticides in surface and ground waters by liquid chromatography-electrospray-tandem mass spectrometry, Anal. Chim. Acta 678(2010) 63-72.
13. [13]
  [13] W. Kanchanamayoon, N. Tatrahun, Determination of polycyclic aromatic hydrocarbons in water samples by solid phase extraction and gas chromatography, World J. Chem. 3(2008) 51-54.
14. [14]
  [14] (Ⅰ). Windal, L. Boxus, V. Hanot, Validation of the analysis of the 15+1 Europeanpriority polycyclic aromatic hydrocarbons by donnor-acceptor complex chromatography and high-performance liquid chromatography-ultraviolet/fluorescence detection, J. Chromatogr. A 1212(2008) 16-22.
15. [15]
  [15] Y.L. Chao, H. Zhou, C.Q. Yu, et al., Determination of PAHs in snow from Hailuogou by C₁₈ membrane extraction chromatography spectrometry, Liaoning Chem. (Ⅰ)nd. 43(2014) 498-502.
16. [16]
  [16] M. (Ⅰ)chihara, A. Yamamoto, K.(Ⅰ). Takakura, N. Kakutani, M. Sudo, Distribution and pollutant load of hexabromocyclododecane (HBCD) in sewage treatment plants and water from Japanese Rivers, Chemosphere 110(2014) 78-84.
17. [17]
  [17] Y. Liu, K. Hu, X.P. Ye, Progress in research of analysis on the hexabromocyclododecane, Guangdong Chem. (Ⅰ)nd. 39(2012) 296-297.
18. [18]
  [18] J. Sánchez-Avila, M. Fernandez-Sanjuan, J. Vicente, S. Lacorte, Development of a multi-residue method for the determination of organic micropollutants in water, sediment and mussels using gas chromatography-tandem mass spectrometry, J. Chromatogr. A 1218(2011) 6799-6811.
19. [19]
  [19] K. Kalachova, J. Pulkrabova, T. Cajka, et al., Gas chromatography-triple quadrupole tandem mass spectrometry:a powerful tool for the (ultra) trace analysis of multiclass environmental contaminants in fish and fish feed, Anal. Bioanal. Chem. 405(2013) 7803-7815.
20. [20]
  [20] Y.J. Wang, L. Li, X.D. Ma, et al., Determination of organochlorine pesticides and PCBs in sea water by silica gel column separation and gas chromatography, Environ. Monitor. China 25(2009) 39-41.
21. [21]
  [21] X.D. Ma, Z.W. Yao, Z. Wang, et al., Distribution and environmental behavior of PAHs in different matrixes on the Fildes Peninsula, Antarctica, Advan. Polar Sci. 26(2014) 285-291.
22. [22]
  [22] X. Wu, G.R. Zu, H. Gao, et al., Distribution characteristic and bioaccumulation of hexabromocyclododecanes (HBCDs) in multimedia environment in the coast of northern Yellow Sea, J. Environ. Chem. 33(2014) 142-147.
23. [23]
  [23] J.P. Chen, Q. Fu, Monitoring Technology of Persistent Organic Pollutants in Water, Chemical (Ⅰ)ndustry Press, Beijing, 2015.
24. [24]
  [24] M.J. Deng, Y.N. Luo, C.B. Deng, Determination of 19 polychlorinated biphenyls in water by gas chromatography-mass spectrometry with solid phase extraction, Chin. J. Spectr. Lab. 29(2012) 947-950.
25. [25]
  [25] S.D. Yu, Determination of polycyclic aromatic hydrocarbons, PCBs, and phthalats by SPE disk extraction-GC/MS with selected ion monitoring mode, Anal. TestingTechnol. (Ⅰ)nstrum. 12(2006) 161-165.
26. [26]
  [26] M. Vecchiato, E. Argiriadis, S. Zambon, et al., Persistent organic pollutants (POPs) in Antarctica:occurrence in continental and coastal surface snow, Microchem. J. 119(2015) 75-82.
27. [27]
  [27] R. Fuoco, S. Giannarelli, M. Onor, et al., A snow/firn four-century record of polycyclic aromatic hydrocarbons (PAHs) and polychlorobiphenyls (PCBs) at Talos Dome (Antarctica), Microchem. J. 105(2012) 133-141.
28. [28]
  [28] E. Martinez, M. Gros, S. Lacorte, D. Barceló, Simplified procedures for the analysis of polycyclic aromatic hydrocarbons in water, sediments and mussels, J. Chromatogr. A 1047(2004) 181-188.
29. [29]
  [29] G.S. Na, C.Y. Liu, Z. Wang, et al., Distribution and characteristic of PAHs in snow of Fildes Peninsula, J. Environ. Sci. 23(2011) 1445-1451.
30. [30]
  [30] Y.F. Wang, F. Liu, Y.M. Sun, F. Shi, Enrichment of trace amount of semi-volatile organic pollutants from large volumes of ground water by extraction with solidphase membrane, Phys. Testing Chem. Anal. 44(2008) 127-130.
31. [31]
  [31] S. Suzuki, A. Hasegawa, Determination of hexabromocyclododecane diastereoisomers and tetrabromobisphenol A in water and sediment by liquid chromatography/mass spectrometry, Anal. Sci. 22(2006) 469-474.
32. [32]
  [32] L.X. Wang, S.H. Qi, X.G. Wu, et al., Spatial and temporal variations of organochlorine pesticides (OCPs) in water and sediments from Honghu Lake, China, J. Geochem. Explor. 132(2013) 181-187.
33. [33]
  [33] D. Yang, S.H. Qi, J.Q. Zhang, et al., Organochlorine pesticides in soil, water and sediment along the Jinjiang River mainstream to Quanzhou Bay, Southeast China, Ecotoxicol. Eniron. Saf. 89(2013) 59-65.
34. [34]
  [34] Y. Hu, S.H. Qi, J.P. Zhang, et al., Assessment of organochlorine pesticides contamination in underground rivers in Chongqing, Southwest China, J. Geochem. Explor. 111(2011) 47-55.
35. [35]
  [35] Y. Yu, Y.X. Li, Z.Y. Shen, et al., Occurrence and possible sources of organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) along the Chao River, China, Chemosphere 114(2014) 136-143.
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