Grasas y Aceites, Vol 71, No 3 (2020)

Solid phase extraction of β-sitosterol and α-tocopherol from sunflower oil deodorizer distillate using desilicated zeolite

O. Karaoglu
The Scientific and Technological Research Council of Turkey - TUBITAK. - Yildiz Technical University, Chemistry Department, Turkey

G. Alpdogan
Yildiz Technical University, Chemistry Department, Turkey

I. S. Ozdemir
The Scientific and Technological Research Council of Turkey - TUBITAK, Turkey

E. Ertas
The Scientific and Technological Research Council of Turkey - TUBITAK, Turkey


In this study, the efficiency of using zeolite-based adsorbents in a solid phase extraction (SPE) procedure of α-tocopherol and β-sitosterol isolation from Sunflower Oil Deodorizer Distillate (SuDOD) with­out pre-treatment was investigated. The results showed that 99.2% α-tocopherol and 97.3% β-sitosterol were suc­cessfully isolated as pure fractions from SuDOD, when desilicated ZSM-5-type zeolite (DSiZSM-5) was used as adsorbent on a SPE. A simple and rapid HPLC method for simultaneous α-tocopherol and β-sitosterol analysis was developed and validated according to AOAC guidelines. It was found that the inclusion of a DSiZSM-5 SPE step increased the precision of the α-tocopherol and β-sitosterol analysis. In conclusion, DSiZSM-5 zeo­lite was proven to be an efficient adsorbent which can be used not only for the recovery of α-tocopherol and β-sitosterol from SuDOD in industrial scale, but also in a laboratory scale clean-up method prior to the analysis of α-tocopherol and β-sitosterol.


SPE; Sterol; Sunflower oil deodorizer distillate; Tocopherol; Zeolite

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Alghamdi EM, Whitcombe MJ, Piletsky SA, Piletska EV. 2018. Solid phase extraction of α-tocopherol and other physi­ologically active components from sunflower oil using rationally designed polymers. Anal. Methods 10, 314–321.

AOAC 2002. AOAC Guidelines for Single Laboratory Validation of Chemical Methods for Dietary Supplements and Botanicals.

Czauderna M, Kowalczyk J, Niedzwiedzka KM. 2009. Simple HPLC Analysis of Tocopherols and Cholesterol from Specimens of Animal Origin. Chem. Anal. (Warsaw) 54, 203–214.

Gaag FJ, Bekkum HV. 1984. Identification of ZSM-type and other 5-rin l containing zeolites by i.r. spectroscopy. Zeolites 4 (4), 369–372.

Gounaris EC, Wei J, Floudas AC. 2008. Shape Selective Zeolite Separation and Catalysis: Optimization Methods. Encyclopedia of Optimization. Springer, Boston, MA.

Ghosh S, Bhattacharyya D. 1996. Isolation of tocopherol and sterol concentrate from sunflower oil deodorizer distil­late. J. Am. Oil Chem. Soc. 73, 1271–1274.

Gunawan S, Ju Y. 2009. Vegetable Oil Deodorizer Distillate: Characterization, Utilization and Analysis. Sep. Purif. Rev. 38, 207–241.

ISO 1999. Animal and vegetable fats and oils – Determination of individual and total sterols contents – Gas chromato­graphic method.

ISO 2016. Animal and vegetable fats and oils – Determination of tocopherol and tocotrienol contents by high-performance liquid chromatography.

Jiang S, Shao P, Pan L, Zhao Y. 2006. Molecular distillation for recovering tocopherol and fatty acid methyl esters from rapeseed oil deodoriser distillate. Biosyst. Eng. 93, 383–391.

Le Van Mao R, Ramsaran A, Xiao S, Yao J, Semmer V. 1995. pH of the Sodium-Carbonate Solution Used for the Desilication of Zeolite Materials. J. Mater. Chem. 5, 533–535.

Li M, Pham PJ, Pittman JCU, Li T. 2008. Selective Solid-Phase Extraction of a-Tocopherol by Functionalized Ionic Liquid-modified Mesoporous SBA-15 Adsorbent. Anal. Sci. 24, 1245–1250.

Martins Z, Pinho O, Ferreira I. 2017. Food industry by-products used as functional ingredients of bakery products. Trends Food Sci. Technol. 67, 106–128.

Maya F, Cabello C, Ghani M, Palomino G, Cerda V. 2018. Emerging materials for sample preparation. J. Sep.Sci. 41, 262–287.

Moreira EA, Baltanas, MA. 2004. Recovery of phytoster­ols from sunflower oil deodorizer distillates. J. Am. Oil Chem. Soc. 81, 161–167.

Renzi M, Righi F, Quarantelli C, Quarantelli A, Bonomi A. 2005. Simplified HPLC-UV method for the deter­mination of ±-tocopherol in plasma. Italian Journal of Animal Science 4, 191–195.

Reyes-Garces N, Gionfriddo E, Gomez-Rios G, Alam M, Boyaci E, Bojko B, Singh V, Grandy J, Pawliszyn J. 2018. Advances in Solid Phase Microextraction and Perspective on Future Directions. Anal. Chem. 90, 302–360.

Sheng Y, Chen XB. 2009. Isolation and identification of an isomer of ß-sitosterol by HPLC and GC-MS. Health 1, 203–206.

Silaghi M, Chizallet C, Raybaud P. 2014. Challenges on molecu­lar aspects of dealumination and desilication of zeolites. Microporous Mesoporous Mater. 191, 82–96.

Socaci SA, Farcas AC, Vodnar DC, Tofana M. 2017. Food Wastes as Valuable Sources of Bioactive Molecule. Superfood and Functional Food—The Development of Superfoods and Their Roles as Medicine. Rijeka, Croatia: InTech. 75–93.

Vazquez L, Torres C, Fornari T, Grigelmo N, Senorans F, Reglero G. 2006. Supercritical fluid extraction of minor lipids from pretreated sunflower oil deodorizer distillates. Eur. J. Lipid Sci. and Technol. 108, 659–665.

Verboekend D, Perez-Ramirez J. 2011. Design of hierarchi­cal zeolite catalysts by desilication. Catal. Sci. Technol. 1, 879–890.

Yan F, Yang H, Li J, Wang H. 2012. Optimization of phytoster­ols recovery from soybean oil deodorizer distillate. J. Am. Oil Chem. Soc. 89, 1363–1370.

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