Development of a Dispersive Liquid–Liquid Microextraction Method for the Determination of α-Tocopherol in Pigmented Wheat by High-Performance Liquid Chromatography
Tóm tắt
A dispersive liquid–liquid microextraction (DLLME) method coupled to high-performance liquid chromatography was developed for the analysis of α-tocopherol in grain samples. The DLLME parameters including the type and volume of extractants, the volume of disperser and the addition of salt were examined. The optimized DLLME procedure consisted in the formation of a cloudy solution promoted by the fast addition to the sample (5 mL of saponified sample solution diluted with 5 mL of water) of a mixture of carbon tetrachloride (extraction solvent, 80 μL) and ethanol (dispersive solvent, 200 μL) without the addition of salt, followed by shaking for 5 min and centrifuging for 3 min at 5,000 rpm. Intra- and inter-day repeatability expressed as % RSD were 3.5 and 7.6 %, respectively. The limit of detection and the limit of quantification were 1.9 and 6.3 μg L−1. The comparison of this method with the national standardized extraction method, supercritical carbon dioxide extraction, accelerated solvent extraction, and conventional heat-reflux extraction indicates that the DLLME was accurate (no significant differences at the 0.05 % probability level), high efficient, low organic solvent-consuming, and low cost. This procedure was successfully applied to 42 samples of 14 types of purple wheat, for which the content of α-tocopherol exhibited a significantly negative correlation with the pigment content measured by a spectrophotometer. The recovery rates ranged from 90.5 to 103.7 %.
Tài liệu tham khảo
Abdel-Aal ES M, Hucl P (1999) A rapid method for quantifying total anthocyanins in blue aleurone and purple pericarp wheats. Cereal Chem 76:350
Bai YF, Hou BY, Sun SC, Sun Y, Pei ZY, Yan GY (2002) Genetic differences of gliadin profiles of black-grained wheat germplasm resources. J Triticeae Crop 22:22
Bustamante-Rangel M, Delgado-Zamarreño M, Sánchez-Pérez A, Carabias-Martínez R (2007) Determination of tocopherols and tocotrienols in cereals by pressurized liquid extraction–liquid chromatography–mass spectrometry. Anal Chim Acta 587:216
Chávez-Servín JL, Castellote AI, López-Sabater MC (2008) Vitamins A and E content in infant milk-based powdered formulae after opening the packet. Food Chem 106:299
Chen HX, Chen H, Ying J, Huang JL, Liao L (2009) Dispersive liquid–liquid microextraction followed by high-performance liquid chromatography as an efficient and sensitive technique for simultaneous determination of chloramphenicol and thiamphenicol in honey. Anal Chim Acta 632:80
De Pascual-Teresa S, Santos-Buelga C, Rivas-Gonzalo JC (2002) LC–MS analysis of anthocyanins from purple corn cob. J Sci Food Agr 82:1003
Escribano-Bailón MT, Santos-Buelga C, Rivas-Gonzalo JC (2004) Anthocyanins in cereals. J Chromatogr A 1054:129
Farahani H, Norouzi P, Dinarvand R, Ganjali MR (2007) Development of dispersive liquid–liquid microextraction combined with gas chromatography–mass spectrometry as a simple, rapid and highly sensitive method for the determination of phthalate esters in water samples. J Chromatogr A 1172:105
Guo L, Lee HK (2011) Ionic liquid based three-phase liquid–liquid–liquid solvent bar microextraction for the determination of phenols in seawater samples. J Chromatogr A 1218:4299
Gao XY, Ran HH, Wang C, Qin XL, Lu ZP (2006) Analysis of part quality traits of Nanyang special color wheat. J Triticeae Crop 26:161
Ge YQ, Yan H, Hui BD, Ni YY, Wang SX, Cai T (2002) Extraction of natural vitamin E from wheat germ by supercritical carbon dioxide. J Agric Food Chem 50:685
Hejtmánková K, Lachman J, Hejtmánková A, Pivec V, Janovská D (2010) Tocols of selected spring wheat (Triticum aestivum L.), einkorn wheat (Triticum monococcum L.) and wild emmer (Triticum dicoccum Schuebl [Schrank]) varieties. Food Chem 123:1267
Hosomi A, Arita M, Sato Y, Kiyose C, Ueda T, Igarashi O, Arai H, Inoue K (1997) Affinity for α-tocopherol transfer protein as a determinant of the biological activities of vitamin E analogs. FEBS Lett 409:105
Hu C, Cai YZ, Li WD, Corke H, Kitts DD (2007) Anthocyanin characterization and bioactivity assessment of a dark blue grained wheat (Triticum aestivum L. cv. Hedong Wumai) extract. Food Chem 104:955
Hu C, Zawistowski J, Ling WH, Kitts DD (2003) Black rice (Oryza sativa L. indica) pigmented fraction suppresses both reactive oxygen species and nitric oxide in chemical and biological model systems. J Agric Food Chem 51:5271
Hussain A, Larsson H, Olsson ME, Kuktaite R, Grausgruber H, Johansson E (2012) Is organically produced wheat a source of tocopherols and tocotrienols for health food? Food Chem 132:1789
Irakli MN, Samanidou VF, Papadoyannis IN (2012) Optimization and validation of the reversed-phase high-performance liquid chromatography with fluorescence detection method for the separation of tocopherol and tocotrienol isomers in cereals, employing a novel sorbent material. J Agric Food Chem 60:2076
Knievel DC, Abdel-Aal ESM, Rabalski I, Nakamura T, Hucl P (2009) Grain color development and the inheritance of high anthocyanin blue aleurone and purple pericarp in spring wheat (Triticum aestivum L.). J Cereal Sci 50:113
Lampi AM, Nurmai T, Ollilainen V, Piironen V (2008) Tocopherols and tocotrienols in wheat genotypes in the HEALTHGRAIN diversity screen. J Agric Food Chem 56:9716
Lanina SA, Toledo P, Sampels S, Eldin AK, Jastrebova JA (2007) Comparison of reversed-phase liquid chromatography–mass spectrometry with electrospray and atmospheric pressure chemical ionization for analysis of dietary tocopherols. J Chromatogr A 1157:159
Li XP, Hou HJ, Liu YP, Lan SQ, Zhe YY (2002) Studies of grain nutritional quality on wheat with blue or purple kernels. Acta Agric Boreali-Sin 17:21
Li ZS, Mu SM, Jiang LX, Zhou HP, Wu JK, Yu L (1982) Study on blue-grained monosomie wheat (1). Acta Genatica Sin 9:431
Li W, Shan F, Sun SC, Corke H, Beta T (2005) Free radical scavenging properties and phenolic content of Chinese black-grained wheat. J Agric Food Chem 53:8533
Liang P, Xu J, Li Q (2008) Application of dispersive liquid–liquid microextraction and high-performance liquid chromatography for the determination of three phthalate esters in water samples. Anal Chim Acta 609:53
Liu YP, Quan SY, Li XP, Lan SQ, Liu YH, Li JP (2002) Protein content and acid composition and qualities of different blue or purple grain wheat. Acta Agric Boreali-Sin 17:103
Mu SM, Li ZS, Zhou HP, Yu L (1986) Cytogenetic identification on blue-grained wheat. Acta Genatica Sin 13:259
National Standard of the People’s Republic of China, GB/T 5009.82-2003, Method for determination of retinol and tocopherol in food
Ortiz-Monasterio JI, Palacios-Rojas N, Meng E, Pixley K, Trethowan R, Peña RJ (2007) Enhancing the mineral and vitamin content of wheat and maize through plant breeding. J Cereal Sci 46:293
Pinheiro-Sant’Ana HM, Guinazi M, Oliveira DS, Lucia CMD, Reis BL, Brandão SCC (2011) Method for simultaneous analysis of eight vitamin E isomers in various foods by high performance liquid chromatography and fluorescence detection. J Chromatogr A 1218:8496
Ryynanen M, Lampi AM, Salo-Vaananen P, Ollilainen V, Piironen V (2004) A small-scale sample preparation method with HPLC analysis for determination of tocopherols and tocotrienols in cereals. J Food Compos Anal 17:749
Rezaee M, Assadi Y, Hosseini MR, Elham A, Fardin A, Sana B (2006) Determination of organic compounds in water using dispersive liquid–liquid microextraction. J Chromatogr A 1116:1
Rezaee M, Yamini Y, Faraji M (2010) Evolution of dispersive liquid–liquid micro-extraction method. J Chromatogr A 1217:2342
Sun SC, Sun Y, Yuan WY, Yan WZ, Pei ZY, Zhang MR, Bai YF (1999) Breeding and qualitative analysis for blank grain wheat 76 of superior quality. Acta Agron Sin 25:50
Shu MW, Leong MI, Fuh MR, Huang SD (2012) Determination of endocrine-disrupting phenols in water samples by a new manual shaking-enhanced, ultrasound-assisted emulsification microextraction method. Analyst 137:2143
Theriault A, Chao JT, Wang Q, Gapor A, Adeli K (1999) Tocotrienol: a review of its therapeutic potential. Clin Biochem 32:303
Xiu Y, Zhao SC, Wang XZ (2009) Determination of vitamin E contents and its correlation with pigment contents in wheat varieties with different seed color. J Triticeae Crop 29:608
Zang XH, Wu QH, Zhang MY, Xi GH, Wang Z (2009) Developments of dispersive liquid–liquid microextraction technique. Chin J Anal Chem 37:161
Zhou K, Laux JJ, Yu L (2004) Comparison of Swiss red wheat grain and fractions for their antioxidant properties. J Agric Food Chem 52:1118
Zhou QX, Pang L, Xiao JP (2009) Trace determination of dichlorodiphenyltri-chloroethane and its main metabolites in environmental water samples with dispersive liquid–liquid microextraction in combination with high performance liquid chromatography and ultraviolet detector. J Chromatogr A 1216:6680
Zhou CH, Tong SS, Chang YX, Jia Q, Zhou WH (2012) Ionic liquid-based dispersive liquid–liquid microextraction with back-extraction coupled with capillary electrophoresis to determine phenolic compounds. Electrophoresis 33:1331