Determination of three chlorophenols in red wine by sweeping-micellar electrokinetic chromatography coupled with dispersive liquid-liquid microextraction and reversed phase liquid-liquid microextraction

doi:10.3724/SP.J.1123.2013.11004

Abstract

Abstract:

A method of dispersive liquid-liquid microextraction (DLLME) and reversed phase liquid-liquid microextraction (RP-LLME) procedures coupled with sweeping-micellar electrokinetic chromatography (sweeping-MEKC) was established to extract and determine the three chlorophenols (CPs) including pentachlorophenol (PCP), 2,4,6-trichlorophenol (TCP) and 2,4-dichlorophenol (DCP) in red wine. The influences of the parameters of two extraction steps and the electrophoresis conditions were investigated. The optimum extraction conditions were as follows: for DLLME, 3.5 mL red wine sample (pH 3.0, 120 g/L NaCl), 300 μL hexane (extraction solvent), extraction for 3 min, centrifugation for 3 min at 5000 r/min; for RP-LLME, 25 μL 0.16 mol/L NaOH solution, extraction for 2 min, centrifugation for 2 min at 5000 r/min. The optimum running buffer (pH 2.3) was an aqueous solution containing 25 mmol/L NaH₂PO₄, 100 mmol/L sodium dodecyl sulfate (SDS) and 30% (v/v) acetonitrile. The optimum on-line concentration conditions were as follows: sample matrix, 80 mmol/L NaH₂PO₄; hydrodynamic injection of 20 s at 20.67 kPa (3 psi). Under the optimum conditions, the excellent linearity was obtained over the range of 0.5-100 μg/L (r≥0.9910) for PCP and TCP, and 1.5-80 μg/L (r≥0.9851) for DCP. The limits of detection (S/N=3) were in the range of 0.035-0.114 μg/L. The average recoveries were in the range of 75.2%-104.7% with the relative standard deviations (RSDs) not more than 6.17%. The results indicated that the proposed method may find wide applications for the determination of trace CPs in various sample matrixes and other weak acidic organic contaminants.

Key words: chlorophenols (CPs), dispersive liquid-liquid microextraction (DLLME), micellar electrokinetic chromatography (MEKC), red wine, reversed phase liquid-liquid microextraction (RP-LLME), sweeping

CLC Number:

O658

SUN Jianzhi, HE Hui, LIU Shuhui. Determination of three chlorophenols in red wine by sweeping-micellar electrokinetic chromatography coupled with dispersive liquid-liquid microextraction and reversed phase liquid-liquid microextraction[J]. Chinese Journal of Chromatography, 2014, 32(3): 256-262.

References

[1] Morales S, Canosa P, Rodriguez I, et al. J Chromatogr A, 2005, 1082(2): 128
[2] Padilla-Sanchez J A, Plaza-Bolanos P, Romero-Gonzalez R, et al. J Chromatogr A, 2010, 1217(14): 5724
[3] Gao X J, Zhang Y, Sun S P. Chinese Journal of Health Laboratory Technology (高学杰, 张毅, 孙仕萍. 中国卫生检验杂质), 2011, 21(5): 1098
[4] Campillo N, Vinas P, Cacho J I, et al. J Chromatogr A, 2010, 1217(47): 7323
[5] Pizarro C, Saenz-Gonzalez C, Perez-del-Notario N, et al. J Chromatogr A, 2010, 1217(49): 7630
[6] Rodriguez I, Cela R. Trends Anal Chem, 1997, 16(8): 463
[7] Ying L C, Ouyang W H. Industrial Water & Wastewater (应立春, 欧阳文华. 工业用水与废水), 2013, 44(4): 86
[8] Minuti L, Pellegrino R M, Tesei I. J Chromatogr A, 2006, 1114(2): 263
[9] Li H Y, Zhang Q, Kang S Y, et al. Chinese Journal of Chromatography (李海玉, 张庆, 康苏媛, 等. 色谱), 2012, 30(6): 596
[10] Ho T T, Chen C Y, Li Z G, et al. Anal Chim Acta, 2012, 712: 72
[11] Holopainen S, Luukkonen V, Nousiainen M, et al. Talanta, 2013, 114: 176
[12] Rezaee M, Assadi Y, Hosseini M M, et al. J Chromatogr A, 2006, 1116(1/2): 1
[13] Hashemi P, Raeisi F, Ghiasvand A R, et al. Talanta, 2010, 80(5): 1926
[14] Xiao C Q, Tang M Q, Li J, et al. J Chromatogr B, 2013, 931(15): 111
[15] Hadjmohammadi M R, Fatemi M H, Shakeri P. J Sep Sci, 2012, 35(1): 3375
[16] Moradi M, Yamini Y, Esrafili A, et al. Talanta, 2010, 82(5): 1864
[17] Us M F, Alshana U, Lubbad I, et al. Electrophoresis, 2013, 34(6): 854
[18] Monton M R N, Imami K, Nakanishi M, et al. J Chromatogr A, 2005, 1079(1/2): 266
[19] Zhang S H, Yang X M, Yin X F, et al. Food Chem, 2013, 133(2): 544
[20] Liu S Q, Wang H L. Chinese Journal of Chromatography (刘胜权, 汪海林. 色谱), 2011, 29(9): 816
[21] Lu Y C, Wang H Y, Song P P, et al. Chinese Journal of Chromatography (卢玉超, 王海燕, 宋萍萍, 等. 色谱), 2011, 29(11): 1122
[22] Dawod M, Breadmore M C, Guijt R M, et al. J Chromatogr A, 2010, 1217(3): 386
[23] Li D L, Guo Y Y, Chang Z X, et al. J Chem Eng Data, 2013 58(3): 731
[24] Galan-Cano F, Lucena R, Cardenas S, et al. J Chromatogr A, 2012, 1229(16): 48
[25] Li X Y, Xue A F, Chen H, et al. J Chromatogr A, 2013, 1280(1): 9
[26] Morais P D, Stoichev T, Basto M P, et al. Talanta, 2012, 89(1): 1
[27] Zhou C H, Tong S S, Chang Y X, et al. Electrophoresis, 2012, 33(8): 1331
[28] Liang T T, Lv Z H, Jiang T F, et al. Electrophoresis, 2013, 34(3): 345
[29] GB 5749-2006