Abstract
We have developed a method, termed solidification of floating organic drop microextraction (SFOME), for the extraction of polybrominated diphenyl ethers (PBDEs) in water and urine samples, this followed by quantification via HPLC. This method requires very small quantities of organic solvent consumption. It is based on exposing a floating solidified drop of an organic solvent on the surface of aqueous solution in a sealed vial. The organic drop is easily collected with a spatula, molten (at ambient temperature), and then submitted to HPLC. Experimental parameters including extraction solvent and its volume, disperser solvent and its volume, extraction time, ionic strength, stirring speed and extraction temperature were optimized. The enrichment factors of analytes are in the range from 921 to 1,462, and acceptable extraction recoveries (92%–118%) are obtained. The dynamic linear range for five PBDE congeners is in the range of 0.5–75 μg.L−1 and from 5 to 500 μg.L−1 for BDE 209. The correlation coefficients range from 0.9960 to 0.9999. The limits of detection (at S/N = 3) for PBDE congeners vary between 0.01 and 0.04 μg.L−1. This method has been successfully applied to detecting PBDEs in two environmental waters and in human urine.
Similar content being viewed by others
References
Dufault C, Poles G, Driscoll LL (2005) Brief postnatal PBDE exposure alters learning and the cholinergic modulation of attention in rats. Toxicol Sci 88:172–180
Kodavanti PR, Ward TR, Ludewig G, Robertson LW, Birnbaum LS (2005) Polybrominated diphenyl ether (PBDE) effects in rat neuronal cultures: 14C-PBDE accumulation, biological effects, and structure-activity relationships. Toxicol Sci 88:181–192
Viberg H, Fredriksson A, Eriksson P (2005) Deranged spontaneous behaviour and decrease in cholinergic muscarinic receptors in hippocampus in the adult rat, after neonatal exposure to the brominated flame-retardant, 2,2′,4,4′,5-pentabromodiphenyl ether (PBDE 99). Environ Toxicol Pharmacol 20:283–288
Fernie KJ, Mayne G, Shutt JL, Pekarik C, Grasman KA, Letcher RJ, Drouillard K (2005) Evidence of immunomodulation in nestling American kestrels (Falco sparverius) exposed to environmentally relevant PBDEs. Environ Pollut 138:485–493
Nakari T, Pessala P (2005) In vitro estrogenicity of polybrominated flame retardants. Aquat Toxicol 74:272–279
Tseng LH, Li MH, Tsai SS, Lee CW, Pan MH, Yao WJ, Hsu PC (2008) Developmental exposure to decabromodiphenyl ether (PBDE 209): effects on thyroid hormone and hepatic enzyme activity in male mouse offspring. Chemosphere 70:640–647
Costa LG, Giordano G (2007) Developmental neurotoxicity of polybrominated diphenyl ether (PBDE) flame retardants. Neurotoxicology 28:1047–1067
KemmLein S, Herzke D, Law RJ (2003) BFR-governmental testing programme. Environ Int 29:781–792
Hyötyläinen T, Hartonen K (2002) Determination of brominated flame retardants in environmental samples. Trends Anal Chem 21:13–30
Cheung KC, Poon BH, Lan CY, Wong MH (2003) Assessment of metal and nutrient concentrations in river water and sediment collected from the cities in the Pearl River Delta, South China. Chemosphere 52:1431–1440
Zheng GJ, Martin M, Richardson BJ, Yu H, Liu Y, Zhou C, Li J, Hu G, Lam MH, Lam PK (2004) Concentrations of polybrominated diphenyl ethers (PBDEs) in Pearl River Delta sediments. Mar Pollut Bull 49:514–524
Li Y, Hu J, Liu X, Fu L, Zhang X, Wang X (2008) Dispersive liquid-liquid microextraction followed by reversed phase HPLC for the determination of decabrominated diphenyl ether in natural water. J Sep Sci 31:2371–2376
Pan J, Yang YL, Xu Q, Chen DZ, Xi DL (2007) PCBs, PCNs and PBDEs in sediments and mussels from Qingdao coastal sea in the frame of current circulations and influence of sewage sludge. Chemosphere 66:1971–1982
Cai ZW, Jiang GB (2006) Determination of polybrominated diphenyl ethers in soil from e-waste recycling site. Talanta 70:88–90
Päpke O, Fürst P, Herrmann T (2004) Determination of polybrominated diphenylethers (PBDEs) in biological tissues with special emphasis on QC/QA measures. Talanta 63:1203–1211
Akutsu K, Obana H, Okihashi M, Kitagawa M, Nakazawa H, Matsuki Y, Makino T, Oda H, Hori S (2001) GC/MS analysis of polybrominated diphenyl ethers in fish collected from the inland sea of Seto, Japan. Chemosphere 44:1325–1333
She J, Holden A, Sharp M, Tanner M, Williams-Derry C, Hooper K (2007) Polybrominated diphenyl ethers (PBDEs) and polychlorinated biphenyls (PCBs) in breast milk from the Pacific Northwest. Chemosphere 67:S307–S317
Pirard C, De Pauw E (2007) Absorption, disposition and excretion of polybrominated diphenyl ethers (PBDEs) in chicken. Chemosphere 66:320–325
Serôdio P, Cabral MS, Nogueira JM (2007) Use of experimental design in the optimization of stir bar sorptive extraction for the determination of polybrominated diphenyl ethers in environmental matrices. J Chrom A 1141:259–270
Prieto A, Zuloaga O, Usobiaga A, Etxebarria N, Fernández LA (2008) Use of experimental design in the optimisation of stir bar sorptive extraction followed by thermal desorption for the determination of brominated flame retardants in water samples. Anal Bioanal Chem 390:739–748
Martínez A, Ramil M, Montes R, Hernanz D, Rubí E, Rodríguez I, Cela Torrijos R (2004) Development of a matrix solid-phase dispersion method for the screening of polybrominated diphenyl ethers and polychlorinated biphenyls in biota samples using gas chromatography with electron-capture detection. J Chrom A 1072:83–91
Wang JX, Jiang DQ, Gu ZY, Yan XP (2006) Multiwalled carbon nanotubes coated fibers for solid-phase microextraction of polybrominated diphenyl ethers in water and milk samples before gas chromatography with electron-capture detection. J Chrom A 1137:8–14
Bayen S, Lee HK, Obbard JP (2004) Determination of polybrominated diphenyl ethers in marine biological tissues using microwave-assisted extraction. J Chrom A 1035:291–294
Li YY, Wei GH, Hu J, Liu XJ, Zhao XN, Wang XD (2008) Dispersive liquid–liquid microextraction followed by reversed phase-high performance liquid chromatography for the determination of polybrominated diphenyl ethers at trace levels in landfill leachate and environmental water samples. Anal Chim Acta 615:96–103
Rezaei F, Bidari A, Birjandi AP, Milani Hosseini MR, Assadi Y (2008) Development of a dispersive liquid-liquid microextraction method for the determination of polychlorinated biphenyls in water. J Hazard Mater 158:621–627
Rezaee M, Assadi Y, Milani Hosseini MR, Aghaee E, Ahmadi F, Berijani S (2006) Determination of organic compounds in water using dispersive liquid-liquid microextraction. J Chrom A 1116:1–9
Berijani S, Assadi Y, Anbia M, Milani Hosseini MR, Aghaee E (2006) Dispersive liquid-liquid microextraction combined with gas chromatography-flame photometric detection: very simple, rapid and sensitive method for the determination of organophosphorus pesticides in water. J Chrom A 1123:1–9
Naseri MT, Hosseini MR, Assadi Y, Kiani A (2008) Rapid determination of lead in water samples by dispersive liquid-liquid microextraction coupled with electrothermal atomic absorption spectrometry. Talanta 75:56–62
Shokoufi N, Shemirani F, Assadi Y (2007) Fiber optic-linear array detection spectrophoto- metry in combination with dispersive liquid-liquid microextraction for simultaneous preconcentration and determination of palladium and cobalt. Anal Chim Acta 597:349–356
Lv LL, Xu H, Song D, Cui Y, Hu S, Zhang G (2010) Analysis of volatile aldehyde biomarkers in human blood by derivatization and dispersive liquid-liquid microextraction based on solidification of floating organic droplet method by high performance liquid chromatography. J Chrom A 1217:2365–2370
Khalili Zanjani MR, Yamini Y, Shariati S, Jönsson JA (2007) A new liquid-phase microextraction method based on solidification of floating organic drop. Anal Chim Acta 585:286–293
Khalili-Zanjani MR, Yamini Y, Yazdanfar N, Shariati S (2008) Extraction and determination of organophosphorus pesticides in water samples by a new liquid phase microextraction gas chromatography-flame photometric detection. Anal Chim Acta 606:202–208
Chang C, Huang S (2010) Determination of the sterod hormone levels in water samples by dispersive liquid-liquid microextraction with solidification of a floating organic drop followed by high performance liquid chromatography. Anal Chim Acta 662:39–43
Li YY, Wei GH, Wang XD (2007) Determination of decabromodiphenyl ether in water samples by single-drop microextraction and RP-HPLC. J Sep Sci 30:2698–2702
Cortazar E, Zuloaga O, Sanz J, Raposo JC, Etxebarria N, Fernández LA (2002) Multisimplex optimization of the solid-phase microextraction gas chromatographic-mass spectrometric determination of polycyclic aromatic hydrocarbons, polychlorinated biphenyls and phthalates from water samples. J Chrom A 978:165–175
Acknowledgements
This work was jointly funded by “Xinmiao Talent” Project of Zhejiang Province (2010R413061), Public Benefit Project of Zhejiang Province (2011C23112, 2011C37006), National Natural Science Foundation of China (21077079), Key Project of Wenzhou City (20082780125, Z090921421), and International Cooperation Project of Wenzhou Science and Technology Bureau (H20090079, H20100053, H20100054).
Author information
Authors and Affiliations
Corresponding authors
Electronic supplementary material
Below is the link to the electronic supplementary material.
ESM 1
(DOC 4286 kb)
Rights and permissions
About this article
Cite this article
Liu, H., Zhang, M., Wang, X. et al. Extraction and determination of polybrominated diphenyl ethers in water and urine samples using solidified floating organic drop microextraction along with high performance liquid chromatography. Microchim Acta 176, 303–309 (2012). https://doi.org/10.1007/s00604-011-0713-1
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s00604-011-0713-1