Skip to main content
SpringerLink
Log in

Simultaneous Determination of Free Phytosterols and Tocopherols in Vegetable Oils by an Improved SPE–GC–FID Method

  • Published:
Food Analytical Methods Aims and scope Submit manuscript

Abstract

In this work, a simple and rapid SPE–GC–FID method for simultaneous determination of free tocopherols and phytosterols in vegetable oils was developed. The use of this SPE approach for the extraction of naturally occurring tocopherols and phytosterols provides advantages such as simplicity, high speed, and ease of use. The whole method was validated, and the limits of detection of tocopherols and phytosterols were 0.05 and 0.03 mg/100 g of oil, respectively. The precisions for the determination of tocopherols and phytosterols in vegetable oils were < 10.1% in relative standard deviations. The recoveries of selected tocopherols and phytosterols spiked at low, middle, and high concentrations ranged from 83.4 to 97.7%. The developed approach was successfully applied to the analysis of free tocopherols and phytosterols in rapeseed, sunflower seed, linseed, sesame, and maize oils.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2

Similar content being viewed by others

References

  • Abidi SL (2001) Chromatographic analysis of plant sterols in foods and vegetable oils. J Chromatogr A 935:173–201

    Article  CAS  Google Scholar 

  • AbuMweis SS, Marinangeli CPF, Frohlich J, Jones PJH (2014) Implementing phytosterols into medical practice as a cholesterol-lowering strategy: overview of efficacy, effectiveness, and safety. Can J Cardiol 30:1225–1232

    Article  Google Scholar 

  • Amaral JS, Casal S, Torres D, Seabra RM, Oliveira BPP (2005) Simultaneous determination of tocopherols and tocotrienols in hazelnuts by a normal phase liquid chromatographic. Anal Sci 21:1545–1548

    Article  CAS  Google Scholar 

  • Araujo P (2009) Key aspects of analytical method validation and linearity evaluation. J Chromatogr B 877:2224–2234

    Article  CAS  Google Scholar 

  • Bakre SM, Gadmale DK, Toche RB, Gaikwad VB (2015) Rapid determination of alpha tocopherol in olive oil adulterated with sunflower oil by reversed phase high-performance liquid chromatography. J Food Sci Technol 52:3093–3098

    Article  CAS  Google Scholar 

  • Bele C, Matea CT, Raducu C, Miresan V, Negrea O (2013) Tocopherol content in vegetable oils using a rapid HPLC fluorescence detection method. Not Bot Horti Agrobot Cluj-Na 41:93–96

    Article  CAS  Google Scholar 

  • Cert A, Moreda W, Pérez-Camino MC (2000) Chromatographic analysis of minor constituents in vegetable oils. J Chromatogr A 881:131–148

    Article  CAS  Google Scholar 

  • Delgado-Zamarreno MM, Fernandez-Prieto C, Bustamante-Rangel M, Perez-Martin L (2016) Determination of tocopherols and sitosterols in seeds and nuts by QuEChERS-liquid chromatography. Food Chem 192:825–830

    Article  CAS  Google Scholar 

  • Esche R, Scholz B, Engel K-H (2013) Online LC–GC Analysis of free sterols/stanols and intact steryl/stanyl esters in cereals. J Agric Food Chem 61:10932–10939

    Article  CAS  Google Scholar 

  • Gliszczyńska-Świgło A, Sikorska E, Khmelinskii I, Sikorski M (2007) Tocopherol content in edible plant oils. Pol J Food Nutr Sci 57:157–161

  • Grilo EC, Costa PN, Gurgel CSS, Beserra AF, Almeida FN, Dimenstein R (2014) Alpha-tocopherol and gamma-tocopherol concentration in vegetable oils. Food Sci Technol 34:379–385

    Article  Google Scholar 

  • Gu Q, Yi XJ, Shen JL, Shi J, Liu YJ, Shao JD (2016) A highly automated method for simultaneous determination of sterols, erythrodiol and uvaol in olive oils. Anal Methods 8:4022–4027

    Article  CAS  Google Scholar 

  • Guan F et al (2012) delta- and gamma-tocopherols, but not alpha-tocopherol, inhibit colon carcinogenesis in azoxymethane-treated F344 rats. Cancer Prev Res (Phila) 5:644–654

    Article  CAS  Google Scholar 

  • Gwatidzo L, Botha BM, McCrindle RI, Combrinck S (2014) Extraction and identification of phytosterols in manketti (Schinziophyton rautanenii) nut oil. J Am Oil Chem Soc 91:783–794

    Article  CAS  Google Scholar 

  • Hennion M-C (1999) Solid-phase extraction: method development, sorbents, and coupling with liquid chromatography. J Chromatogr A 856:3–54

    Article  CAS  Google Scholar 

  • Hu Y, Xiong L, Huang W, Cai H, Luo Y, Zhang Y, Lu B (2014) Anti-inflammatory effect and prostate gene expression profiling of steryl ferulate on experimental rats with non-bacterial prostatitis. Food Funct 5:1150–1159

    Article  CAS  Google Scholar 

  • ICH (2005) Validation of analytical procedures: text and methodology Q2(R1). International Conference on Harmonization (ICH). https://database.ich.org/sites/default/files/Q2_R1__Guideline.pdf

  • Jerzykiewicz M, Ćwieląg-Piasecka I, Jezierski A (2013) Pro- and antioxidative effect of α-tocopherol on edible oils, triglycerides and fatty acids. J Am Oil Chem Soc 90:803–811

    Article  CAS  Google Scholar 

  • Law M (2000) Plant sterol and stanol margarines and health. Br Med J 320:861–864

    Article  CAS  Google Scholar 

  • Lechner M, Reiter B, Lorbeer E (1999) Determination of tocopherols and sterols in vegetable oils by solid-phase extraction and subsequent capillary gas chromatographic analysis. J Chromatogr A 857:231–238

    Article  CAS  Google Scholar 

  • Li GX, Lee MJ, Liu ANB, Yang ZH, Lin Y, Shih WCJ, Yang CS (2011) delta-tocopherol is more active than alpha- or gamma-tocopherol in inhibiting lung tumorigenesis in vivo. Cancer Prev Res (Phila) 4:404–413

    Article  CAS  Google Scholar 

  • Lukić M, Lukić I, Krapac M, Sladonja B, Piližota V (2013) Sterols and triterpene diols in olive oil as indicators of variety and degree of ripening. Food Chem 136:251–258

    Article  Google Scholar 

  • Moreau RA, Whitaker BD, Hicks KB (2002) Phytosterols, phytostanols, and their conjugates in foods: structural diversity, quantitative analysis, and health-promoting uses. Prog Lipid Res 41:457–500

    Article  CAS  Google Scholar 

  • Nestola M, Schmidt TC (2016) Fully automated determination of the sterol composition and total content in edible oils and fats by online liquid chromatography-gas chromatography-flame ionization detection. J Chromatogr A 1463:136–143

    Article  CAS  Google Scholar 

  • Phillips KM, Ruggio DM, Toivo JI, Swank MA, Simpkins AH (2002) Free and esterified sterol composition of edible oils and fats. J Food Compos Anal 15:123–142

    Article  CAS  Google Scholar 

  • San Andrés MP, Otero J, Vera S (2011) High performance liquid chromatography method for the simultaneous determination of α-, γ- and δ-tocopherol in vegetable oils in presence of hexadecyltrimethylammonium bromide/n-propanol in mobile phase. Food Chem 126:1470–1474

    Article  Google Scholar 

  • Smolarek AK et al (2012) Dietary administration of delta- and gamma-tocopherol inhibits tumorigenesis in the animal model of estrogen receptor-positive, but not HER-2 breast cancer. Cancer Prev Res (Phila) 5:1310–1320

    Article  CAS  Google Scholar 

  • Suttiarporn P, Chumpolsri W, Mahatheeranont S, Luangkamin S, Teepsawang S, Leardkamolkarn V (2015) Structures of phytosterols and triterpenoids with potential anti-cancer activity in bran of black non-glutinous rice. Nutrients 7:1672–1687

    Article  CAS  Google Scholar 

  • Xu B, Zhang L, Wang H, Luo D, Li P (2014) Characterization and authentication of four important edible oils using free phytosterol profiles established by GC-GC-TOF/MS. Anal Methods 6:6860–6870

    Article  CAS  Google Scholar 

  • Xu B et al (2015) Detection of virgin coconut oil adulteration with animal fats using quantitative cholesterol by GC x GC–TOF/MS analysis. Food Chem 178:128–135

    Article  CAS  Google Scholar 

  • Xu B et al (2018) Determination of free steroidal compounds in vegetable oils by comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry. Food Chem 245:415–425

    Article  CAS  Google Scholar 

  • Yuan C, Ju Y, Jin R, Ren L, Liu X (2015) Simultaneous HPLC–DAD analysis of tocopherols, phytosterols, and squalene in vegetable oil deodorizer distillates. Chromatographia 78:273–278

    Article  CAS  Google Scholar 

  • Yuan CX, Xie YY, Jin RS, Ren LL, Zhou L, Zhu M, Ju YJ (2017) Simultaneous analysis of tocopherols, phytosterols, and squalene in vegetable oils by high-performance liquid chromatography. Food Anal Methods 10:3716–3722

    Article  Google Scholar 

  • Zhang R et al (2016) Simultaneous determination of tocopherols and tocotrienols in vegetable oils by GC-MS. Anal Methods 8:7341–7346

    Article  CAS  Google Scholar 

Download references

Funding

This work was financially supported by the National Natural Science Foundation of China (31772094), the Natural Science Foundation of Henan Province – China (162300410076), the Doctoral Scientific Research Foundation of Henan University of Science and Technology – China (13480057), and the Graduate Students Innovation Foundation of Henan University of Science and Technology – China (CXJJ-2018-KJ06).

Author information

Author notes

  1. Baocheng Xu and Sicong You contributed equally to this work.

Authors and Affiliations

  1. College of Food and Bioengineering, Henan University of Science and Technology, Luoyang, 471003, China

    Baocheng Xu, Sicong You, Lu Zhou, Huaibin Kang, Denglin Luo, Hongyan Ma & Sihai Han

  2. Henan Engineering Research Center of Food Material, Henan University of Science and Technology, Luoyang, 471003, China

    Baocheng Xu, Huaibin Kang, Denglin Luo & Sihai Han

  3. National Experimental Teaching Demonstration Center of Food Processing and Safety, Henan University of Science and Technology, Luoyang, 471003, China

    Baocheng Xu, Huaibin Kang & Denglin Luo

Authors
  1. Baocheng Xu
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Sicong You
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Lu Zhou
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Huaibin Kang
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Denglin Luo
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. Hongyan Ma
    View author publications

    You can also search for this author in PubMed Google Scholar

  7. Sihai Han
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding authors

Correspondence to Baocheng Xu or Denglin Luo.

Ethics declarations

Conflict of Interest

Baocheng Xu declares that she has no conflict of interest. Sicong You declares that he has no conflict of interest. Lu Zhou declares that she has no conflict of interest. Huaibin Kang declares that she has no conflict of interest. Denglin Luo declares that he has no conflict of interest. Hongyan Ma declares that he has no conflict of interest. Sihai Han declares that he has no conflict of interest.

Ethical Approval

This article does not contain any studies with human or animal subjects.

Informed Consent

Informed consent was obtained from all individual participants included in this study.

Additional information

Publisher’s Note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Xu, B., You, S., Zhou, L. et al. Simultaneous Determination of Free Phytosterols and Tocopherols in Vegetable Oils by an Improved SPE–GC–FID Method. Food Anal. Methods 13, 358–369 (2020). https://doi.org/10.1007/s12161-019-01649-7

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s12161-019-01649-7

Keywords

Search

Navigation