Abstract
We have developed a method for the determination of mercury in water samples that combines dispersive liquid-liquid microextraction (DLLME) with back-extraction (BE) and detection by capillary zone electrophoresis. DLLME is found to be a simple, cost-effective and rapid method for extraction and preconcentration. The BE procedure is based on the fact that the stability constant of the hydrophilic chelate of Hg(II) with L-cysteine is much larger than that of the respective complex with 1-(2-pyridylazo)-2-naphthol. Factors affecting complex formation and extraction efficiency (such as pH value, concentration of the chelating agent, time of ultrasonication and extraction, and type and quantity of disperser solvent) were optimized. Under the optimal conditions, the enrichment factor is 625, and the limit of detection is 0.62 μg L−1. The calibration plot is linear in the range between 1 and 1,000 μg L−1 (R 2 = 0.9991), and the relative standard deviation (RSD, for n = 6) is 4.1%. Recoveries were determined with tap water and seawater spiked at levels of 10 and 100 μg L−1, respectively, and ranged from 86.6% to 95.1%, with corresponding RSDs of 3.95–5.90%.
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References
Rapsomanikis S, Craig PJ (1991) Speciation of mercury and methylmercury compounds in aqueous samples by chromatography atomic-absorption spectrometry after ethylation with sodium tetraethylborate. Anal Chim Acta 248:563–567
Collasiol A, Pozebon D, Maia SM (2004) Ultrasound assisted mercury extraction from soil and sediment. Anal Chim Acta 518:157–164
Wei GT, Yang Z, Chen CJ (2003) Room temperature ionic liquid as a novel medium for liquid/liquid extraction of metal ions. Anal Chim Acta 488:183–192
Provazi K, Campos BA, Espinosa DCR, Tenorio JAS (2011) Metal separation from mixed types of batteries using selective precipitation and liquid-liquid extraction techniques. Waste Manag 31(1):59–64
Bagheri H, Naderi M (2009) Immersed single-drop microextraction-electrothermal vaporization atomic absorption spectroscopy for the trace determination of mercury in water samples. J Hazard Mater 165:353–358
Pena-Pereir F, Lavill I, Bendicho C, Vidal L, Canals A (2009) Speciation of mercury by ionic liquid-based single-drop microextraction combined with high-performance liquid chromatography-photodiode array detection. Talanta 78:537–541
Xia LB, Li X, Wu YL, Hu B, Chen R (2008) Ionic liquids based single drop microextraction combined with electrothermal vaporization inductively coupled plasma mass spectrometry for determination of Co, Hg and Pb in biological and environmental samples. Spectrochim Acta B 63:1290–1296
Jitaru P, Adams FC (2004) Speciation analysis of mercury by solid-phase microextraction and multicapillary gas chromatography hyphenated to inductively coupled plasma-time-of-flight-mass spectrometry. J Chromatogr A 1055:197–207
Mishra S, Tripathi RM, Bhalke S, Shukla VK, Puranik VD (2005) Determination of methylmercury and mercury(II) in a marine ecosystem using solid-phase microextraction gas chromatography-mass spectrometry. Anal Chim Acta 551:192–198
Ructnev A, Spivakov B, Timerbaev A (2000) Solid-phase extraction and subsequent capillary zone electrophoresis of trace metal ions as soluble dithiocarbamate complexes. Chromatographia 52:99–102
Yin Y, Chen M, Peng J-F, Liu J, Jiang G (2010) Dithizone-functionalized solid phase extraction-displacement elution-high performance liquid chromatography-inductively coupled plasma mass spectrometry for mercury speciation in water samples. Talanta 81:1788–1792
Garrido M, Di Nezio MS, Lista AG, Palomeque M, Fernández Band BS (2004) Cloud-point extraction/preconcentration on-line flow injection method for mercury determination. Anal Chim Acta 502:173–177
Yu LP (2005) Cloud point extraction preconcentration prior to high-performance liquid chromatography coupled with cold vapor generation atomic fluorescence spectrometry for speciation analysis of mercury in fish samples. J Agric Food Chem 53:9656–9662
Kubáň P, Houserová P, Kubáň P, Hauser PC, Kubán V (2007) Mercury speciation by CE: a review. Electrophoresis 28:58–68
Kubáň P, Pelcová P, Margetínová J, Kubáň V (2009) Mercury speciation by CE: an update. Electrophoresis 30:92–99
Yildiz A, Lisesivdin SB, Kasap M, Ozcelik S, Ozbay E, Balkan N (2010) Investigation of low-temperature electrical conduction mechanisms in highly resistive GaN bulk layers extracted with simple parallel conduction extraction method. Appl Phys A 98:557–563
Khedhiri S, Semhi K, Duplay J, Darragi F (2011) Comparison of sequential extraction and principal component analysis for determination of heavy metal partitioning in sediments: the case of protected Lagoon El Kelbia (Tunisia). Environ Earth Sci 62(5):1013–1025
Chiou CS, Jiang SJ, Danadurai KSK (2001) Determination of mercury compounds in fish by microwave-assisted extraction and liquid chromatography-vapor generation-inductively coupled plasma mass spectrometry. Spectrochim Acta B 56:1133–1142
Rezaee M, Assadi Y, Hosseini MRM, Aghaee E, Ahmadi F, Berijani S (2006) Determination of organic compounds in water using dispersive liquid-liquid microextraction. J Chromatogr A 1116:1–9
Yamini Y, Rezaeea M, Khanchi A, Faraji M, Saleh A (2010) Dispersive liquid-liquid microextraction based on the solidification of floating organic drop followed by inductively coupled plasma-optical emission spectrometry as a fast technique for the simultaneous determination of heavy metals. J Chromatogr A 1217:2358–2364
Herrera-Herrera AV, Hernández-Borges J, Borges-Miquel TM, Rodríguez-Delgado MÁ (2010) Dispersive liquid-liquid microextraction combined with nonaqueous capillary electrophoresis for the determination of fluoroquinolone antibiotics in waters. Electrophoresis 31:3457–3465
Song XL, Li JH, Liao CY, Chen LX (2011) Ultrasound-assisted dispersive liquid-liquid microextraction combined with little solvent consumption for determination of polycyclic aromatic hydrocarbons in seawater by gas chromatography-mass spectrometry. Chromatographia 74:89–98
Birjandi AP, Bidari A, Rezaei F, Hosseini MRM, Assadi Y (2008) Speciation of butyl and phenyltin compounds using dispersive liquid-liquid microextraction and gas chromatography-flame photometric detection. J Chromatogr A 1193:19–25
Hu J, Fu L, Zhao X, Liu X, Wang H, Wang X, Dai L (2009) Dispersive liquid-liquid microextraction combined with gas chromatography-electron capture detection for the determination of polychlorinated biphenyls in soils. Anal Chim Acta 640:100–105
Zhou Q, Bai H, Xie G, Xiao J (2008) Trace determination of organophosphorus pesticides in environmental samples by temperature-controlled ionic liquid dispersive liquid-phase microextraction. J Chromatogr A 1188:148–153
Tsai WC, Huang SD (2009) Dispersive liquid-liquid-liquid microextraction combined with liquid chromatography for the determination of chlorophenoxy acid herbicides in aqueous samples. J Chromatogr A 1216:7846–7850
Anthemidis AN, Ioannou KIG (2009) On-line sequential injection dispersive liquid-liquid microextraction system for flame atomic absorption spectrometric determination of copper and lead in water samples. Talanta 79:86–91
Naseri MT, Hosseini MRM, 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
Rezaee M, Yamini Y, Khanchi A, Faraji M, Saleh A (2010) A simple and rapid new dispersive liquid-liquid microextraction based on solidification of floating organic drop combined with inductively coupled plasma-optical emission spectrometry for preconcentration and determination of aluminium in water samples. J Hazard Mater 178:766–770
Gharehbaghi M, Shemirani F, Baghdadi M (2009) Dispersive liquid-liquid microextraction based on ionic liquid and spectrophotometric determination of mercury in water samples. Int J Environ Anal Chem 89:21–33
Jia XY, Han Y, Liu XL, Duan TC, Chen HT (2011) Speciation of mercury in water samples by dispersive liquid-liquid microextraction combined with high performance liquid chromatography-inductively coupled plasma mass spectrometry. Spectrochim Acta Part B 66:88–92
Wen YY, Li JH, Zhang WW, Chen LX (2011) Dispersive liquid-liquid microextraction coupled with capillary electrophoresis for simultaneous determination of sulfonamides with the aid of experimental design. Electrophoresis In press, doi: 10.1002/elps.201100142
Almeda S, Gandolfi HE, Arce L, Valcárcel M (2009) Potential of porphyrins as chromogenic reagents for determining metals in capillary electrophoresis. J Chromatogr A 1216:6256–6258
Liu WP, Lee HK (1998) Use of triethylenetetraminehexaacetic acid combined with field amplified sample injection in speciation analysis by capillary electrophoresis. Anal Chem 70:2666–2675
Rudnev A, Spivakov B, Timerbaev A (2000) Solid-phase extraction and subsequent capillary zone electrophoresis of trace metal ions as soluble dithiocarbamate complexes. Chromatographia 52:99–102
Li Y, Jiang Y, Yan XP (2005) On-line hyphenation of capillary electrophoresis with flame-heated furnace atomic absorption spectrometry for trace mercury speciation. Electrophoresis 26:661–667
Li F, Wang DD, Yan XP, Lin JM, Su RG (2005) Development of a new hybrid technique for rapid speciation analysis by directly interfacing a microfluidic chip-based capillary electrophoresis system to atomic fluorescence spectrometry. Electrophoresis 26:2261–2268
Yin XB (2007) Dual-cloud point extraction as a preconcentration and clean-up technique for capillary electrophoresis speciation analysis of mercury. J Chromatogr A 1154:437–443
Kubáň P, Houserová P, Kubáň P, Hauser PC, Kubáň V (2007) Sensitive capillary electrophoretic determination of mercury species with amperometric detection at a copper electrode after cation exchange preconcentration. J Sep Sci 30:1070–1076
Li PJ, Duan JK, Hu B (2008) High-sensitivity capillary electrophoresis for speciation of organomercury in biological samples using hollow fiber-based liquid-liquid-liquid microextraction combined with on-line preconcentration by large-volume sample stacking. Electrophoresis 29:3081–3089
Yan XP, Yin XB, Jiang DQ, He XW (2003) Speciation of mercury by hydrostatically modified electroosmotic flow capillary electrophoresis coupled with volatile species generation atomic fluorescence spectrometry. Anal Chem 75:1726–1732
Sonke JE, Salters VJM (2004) Disequilibrium effects in metal speciation by capillary electrophoresis inductively coupled plasma mass spectrometry (CE-ICP-MS); theory, simulations and experiments. Analyst 129:731–738
Fattahi N, Assadi Y, Hosseini MRM, Jahromi EZ (2007) Determination of chlorophenols in water samples using simultaneous dispersive liquid-liquid microextraction and derivatization followed by gas chromatography-electron-capture detection. J Chromatogr A 1157:23–29
Rezaei F, Bidari A, Birjandi AP, Hosseini MRM, 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
Kozani RR, Assadi Y, Shemirani F, Hosseini MRM, Jamali MR (2007) Part-per-trillion determination of chlorobenzenes in water using dispersive liquid-liquid microextraction combined gas chromatography-electron capture detection. Talanta 72:387–393
Liu W, Lee HK (1998) Simultaneous analysis of inorganic and organic lead, mercury and selenium by capillary electrophoresis with nitrilotriacetic acid as derivatization agent. J Chromatogr A 796:385–395
Chen JG, Chen HW, Jin XZ, Chen HT (2009) Determination of ultra-trace amount methyl-, phenyl- and inorganic mercury in environmental and biological samples by liquid chromatography with inductively coupled plasma mass spectrometry after cloud point extraction preconcentration. Talanta 77:1381–1387
Acknowledgement
This work was financially supported by the National Natural Science Foundation of China (20975089), the Innovation Projects of the Chinese Academy of Sciences (KZCX2-EW-206), the Department of Science and Technology of Shandong Province of China (2008GG20005005), the Natural Science Foundation of Shandong Province of China (ZR2010BQ027), the Science and technology support project of Qingdao Public domain (09-1-1-55-nsh), the Yantai Research and Development Program of China (2010158), and the 100 Talents Program of the Chinese Academy of Sciences.
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Li, J., Lu, W., Ma, J. et al. Determination of mercury(II) in water samples using dispersive liquid-liquid microextraction and back extraction along with capillary zone electrophoresis. Microchim Acta 175, 301–308 (2011). https://doi.org/10.1007/s00604-011-0679-z
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DOI: https://doi.org/10.1007/s00604-011-0679-z