Fatty acid and solidification floating organic drop-based dispersive liquid-liquid microextraction method coupled with high performance liquid chromatography for the determination of 4-ethylphenol and 4-ethylguaiacol in wines

doi:10.3724/SP.J.1123.2016.06021

Abstract

Abstract:

A method of fatty acid and solidification floating organic drop-based dispersive liquid-liquid microextraction (FA-DLLME-SFO) coupled with high performance liquid chromatography to determine 4-ethylphenol (4-EP) and 4-ethylguaiacol (4-EG) in wine samples was developed. The method required less than 4 min to extract the two target analytes from wine samples, and only three kinds of eco-friendly solvents including fatty acid, ammonium hydroxide and sulfuric acid were used. The analytical parameters affecting the extraction efficiency including the volumes of the sample, the nature and volumes of the extraction solvent, the volumes of ammonium hydroxide and sulfuric acid, and the amount of salt addition were optimized. Under the optimum conditions (10 mL sample, 100 μL octanoic acid, 110 μL 25%-28% (mass percentage) NH₄OH, 0.8 mL 98% (mass percentage) H₂SO₄, 3.0 g NaCl), the linear ranges were 0.02-1.0 mg/L with correlation coefficients of 0.9997 and 0.9999 for 4-ethylphenol and 4-ethylguaiacol, and the relative standard deviations (RSDs) were 6.2% and 3.5%, respectively. The LODs were 6.33 μg/L and 5.81 μg/L, and the enrichment factors (EFs) were 79 and 86 for 4-ethylphenol and 4-ethylguaiacol, respectively. The present method was applied to the determination of the two analytes in white wine and beer samples, and the recoveries of them were in the range of 81.4%-108.7% with the RSDs less than 8.9%. The method is simple and eco-friendly for rapid analysis of 4-ethylphenol and 4-ethylguaiacol in wine samples.

Key words: 4-ethylguaiacol (4-EG), 4-ethylphenol (4-EP), dispersive liquid-liquid microextraction (DLLME), fatty acid, high performance liquid chromatography (HPLC)

CLC Number:

O658

FU Bo, ZHANG Jiping, JIANG Hui, ZHOU Lu. Fatty acid and solidification floating organic drop-based dispersive liquid-liquid microextraction method coupled with high performance liquid chromatography for the determination of 4-ethylphenol and 4-ethylguaiacol in wines[J]. Chinese Journal of Chromatography, 2016, 34(9): 895-900.

References

[1] Larcher R, Nicolini G, Puecher C, et al. Anal Chim Acta, 2007, 582: 55
[2] López R, Aznar M, Cacho J, et al. J Chromatogr A, 2002, 966: 167
[3] Domínguez C, Guillén D A, Barroso C G. Anal Chim Acta, 2002, 458: 95
[4] Pizarro C, Sáenz-González C, Pérez-del-Notario N, et al. J Chromatogr A, 2011, 1218: 1576
[5] Pizarro C, Sáenz-González C, Pérez-del-Notario N, et al. J Chromatogr A, 2012, 1244: 37
[6] Rezaee M, Assadi Y, Milani Hosseini M R, et al. J Chromatogr A, 2006, 1116: 1
[7] Leong M I, Huang S D. J Chromatogr A, 2008, 1211: 8
[8] Khalili Zanjani M R, Yamini Y, Shariati S, et al. Anal Chim Acta, 2007, 585: 286
[9] Asadi M, Dadfarnia S, Haji Shabani A M, et al. J Sep Sci, 2015, 38(14): 2510
[10] Asadi M, Haji Shabani A M, Dadfarnia S, et al. Chinese Jounal of Chromatography, 2015, 33 (6): 634 Asadi M, Haji Shabani A M, Dadfarnia S, 等. 色谱, 2015, 33(6): 634
[11] Wang Y, Zhu C H, Zou X L, et al. Chinese Jounal of Chromatography, 2013, 31(11): 1076 王宇, 朱成华, 邹晓莉, 等. 色谱, 2013, 31(11): 1076
[12] Wang J C, Zhang H J, Chen J P, et al. Chinese Jounal of Chromatography, 2014, 32(9): 913 王金成, 张海军, 陈吉平, 等. 色谱, 2014, 32(9): 913
[13] Shih H K, Shu T Y, Ponnusamy V K, et al. Anal Chim Acta, 2015, 854: 70
[14] Vakh C, Pochivalov A, Andruch V, et al. Anal Chim Acta, 2016, 907: 54
[15] Moradi M, Yamini Y, Esrafili A, et al. Talanta, 2010, 82: 1864
[16] Wu C X, Liu N, Wu Q H, et al. Anal Chim Acta, 2010, 679: 56
[17] Bai X H, Hu S, Chen X. Liquid-Phase Microextraction. 1st ed. Beijing: Chemical Industry Press, 2013 白小红, 胡爽, 陈璇. 液相微萃取. 1版. 北京: 化学工业出版社, 2013
[18] Diez J, Dominguez C, Guilend D A, et al. J Chromatogr A, 2004, 1025: 263
[19] Peng Q R, Dong R, Xun S, et al. Flavour Fragr J, 2013, 28: 137
[20] Valente I M, Santos C M, Moreira M M, et al. J Chromatogr A, 2013, 1271: 27
[21] Carpinteiro I, Abuín B, Rodríguez I, et al. J Chromatogr A, 2012, 1229: 79