Determination of eight polybrominated diphenyl ethers in marine sediments by ultrasonically assisted alkaline degradation extraction and gas chromatography- electron capture detection

doi:10.3724/SP.J.1123.2015.04025

Abstract

Abstract:

For determination of the eight polybrominated diphenyl ethers (PBDEs) in marine sediments based on gas chromatography-electron capture detection (GC-ECD), a rapid and effective method for simultaneous sample extraction and purification was developed, in which ultrasonically assisted alkaline hydrolysis was combined with solvent extraction. The sediment sample was processed in an ultrasonic bath in 2.00 mol/L NaOH-methanol solution for 30 min, and subsequently extracted by n-hexane. The organic phase was then separated and purified by silica column and concentrated to 100 μL for GC-ECD analysis. Under the optimized conditions, the recoveries and relative standard deviations (RSDs) for eight PBDE congeners ranged from 63.6% to 110.3% and from 1.7% to 10.5% (n=5), respectively. The limits of detection (LODs, S/N=3) ranged from 0.002 to 0.011 ng/g except for deca-brominated diphenyl ether (BDE-209), which was 0.097 ng/g. With high accuracy, good stability and adequate recovery, the established method was successfully applied to the analysis of PBDEs in the surface sediments from Bohai Sea. The concentrations of ∑₈PBDEs (sum of 2,4,4'-tribromodiphenyl ether (BDE-28), 2,2',4,4'-tetrabromodiphenyl ether (BDE-47), 2,2',4,4',5-pentabromodiphenyl ether (BDE-99), 2,2',4,4',6-pentabromodiphenyl ether (BDE100), 2,2',4,4',5,5'-hexabromodiphenyl ether (BDE-153), 2,2',4,4',5,6'-hexabromodiphenyl ether (BDE-154), 2,2',3,4,4',5',6-heptabromodiphenyl ether (BDE-183), BDE-209) and BDE-209 ranged from 1.566 to 6.760 ng/g and from 1.461 to 6.438 ng/g, respectively. A decreasing gradient of concentration was basically observed with increasing distance off the shore, indicating that anthropogenic activities, surface runoff and river inputs may be the sources of PBDEs in the sediments from Bohai Sea.

Key words: electron capture detection (ECD), gas chromatography (GC), marine sediments, polybrominated diphenyl ethers (PBDEs), ultrasonically assisted alkaline hydrolysis extraction

CLC Number:

O658

WANG Guoguang, ZHANG Dahai, YANG Dandan, PENG Jialin, LI Xianguo. Determination of eight polybrominated diphenyl ethers in marine sediments by ultrasonically assisted alkaline degradation extraction and gas chromatography- electron capture detection[J]. Chinese Journal of Chromatography, 2015, 33(8): 885-891.

References

[1] Huang F F, Li J G, Zhao Y F, et al. Environmental Chemistry (黄飞飞, 李敬光, 赵云峰, 等. 环境化学), 2011, 30(2): 418

[2] Rakkestad K E, Dye C J, Yttri K E, et al. J Environ Monit, 2007, 9(12): 1419

[3] Chen D H, Bi X H, Liu M, et al. Chemosphere, 2011, 82(9): 1246

[4] Qiu X H, Zhu T, Hu J X. Chemosphere, 2010, 80(10): 1207

[5] Nouira T, Risso C, Chouba L, et al. Chemosphere, 2013, 93(3): 487

[6] Frouin H, Lebeuf M, Hammill M, et al. Chemosphere, 2011, 82(5): 663

[7] Rochman C M, Lewison R L, Eriksen M, et al. Sci Total Environ, 2014, 476/477: 622

[8] Hong W, Wei D Y, Dong H M. Chemical Engineering & Equipment (洪伟, 魏东洋, 董洪梅. 化学工程与设备), 2012(12): 150

[9] McDonald T A. Chemosphere, 2002, 46: 745

[10] Chen C E, Zhao H X, Chen J W, et al. Chemosphere, 2012, 88(7): 791

[11] Zou Y M, Ran Y, Gong J, et al. Environ Sci Technol, 2007, 41(24): 8262

[12] Zhou P, Lin K F, Zhou X Y, et al. Chemosphere, 2012, 88(11): 1375

[13] Pan X H, Tang J H, Li J, et al. J Environ Monit, 2010, 12(6): 1234

[14] Li Y Y, Lin T, Chen Y J, et al. Environ Pollut, 2012, 171: 155

[15] Chen L G, Huang Y M, Peng X C, et al. Chemosphere, 2009, 76(2): 226

[16] Chen S J, Mai B X, Zeng Y P, et al. Acta Scientiae Circumstantiae (陈社军, 麦碧闲, 曾永平, 等. 环境科学学报), 2005, 25(9): 1255

[17] You Z Z, Kong D X, Xu J, et al. Environmental Chemistry (由宗政, 孔德祥, 许静, 等. 环境化学), 2013, 32(7): 1410

[18] Wan X, Wang B, Zhao S M, et al. Environmental Chemistry (万幸, 王彬, 赵世民, 等. 环境化学), 2011, 30(10): 1781

[19] Tang Z W, Huang Q F, Cheng J L, et al. Environ Sci Technol, 2014, 48(3): 1508

[20] EPA Method 1668

[21] GB 13015-91

[22] Duan X Y, Li X G, Li Y X, et al. Environmental Chemistry (段晓勇, 李先国, 李艳霞, 等. 环境化学), 2012, 31(10): 1645

[23] Huang F F, Zhao Y F, Li J G, et al. Chinese Journal of Chromatography (黄飞飞, 赵云峰, 李敬光, 等. 色谱), 2011, 29(8): 743

[24] Mai B X, Chen S J, Luo X J, et al. Environ Sci Technol, 2005, 39(10): 3521

[25] Chen S J, Feng A H, He M J, et al. Sci Total Environ, 2013, 444: 205

[26] Chen S J, Gao X J, Mai B X, et al. Environ Pollut, 2006, 144(3): 651

[27] Jiang J J, Lee C L, Fang M D, et al. Mar Pollut Bull, 2011, 62(4): 815

[28] Zhu H, Wang Y, Wang X, et al. Sci Total Environ, 2014, 468: 130

[29] Moon H B, Kannan K, Lee S J, et al. Chemosphere, 2007, 66(2): 243

[30] Song W, Ford J C, Li A, et al. Environ Sci Technol, 2005, 39(15): 5600

[31] Chen S J. [PhD Dissertation]. Guangzhou: Guangzhou Institute of Geochemistry, Chinese Academy of Sciences (陈社军. [博士学位论文]. 广州: 中国科学院广州地球化学研究所), 2005