Journal of the American Oil Chemists' Society

, Volume 89, Issue 9, pp 1577–1584 | Cite as

Ultrahigh Pressure Liquid Chromatographic Determination of Tocopherols in B100 Biodiesel

  • R. E. PaulsEmail author
Original Paper


A reversed-phase gradient ultrahigh pressure liquid chromatographic method with a water–acetonitrile mobile phase and UV detection has been developed to rapidly determine the concentration of the major tocopherol components in B100. The described method requires minimal sample preparation and provides short analysis times compatible with the needs of small to mid-size laboratories involved in B100 analyses. The objectives of this work were twofold. We wished to develop an analytical method both to rapidly screen B100 samples for their tocopherol content and to provide additional information on the source (from the distribution of tocopherols) and the nature of the processing of the B100 (absence of tocopherols would suggest distillation). Information on the tocopherol content of the B100 can be used to assess the inherent antioxidant content of the B100 and the extent to which additional stabilizers are required. The method determines the concentration of alpha, gamma and delta tocopherols and has a chromatographic run time of 4.5 min with minimal sample preparation. Calibration curves were linear over the range of 5–350 μg/mL and had correlation coefficients exceeding 0.999. The short term precision of the method was evaluated, and relative standard deviations were typically 2 % or less. Recovery of spiked tocopherols averaged 97 %.


Tocopherols UPLC Biodiesel 


  1. 1.
    Frohlich A, Schober S (2007) The influence of tocopherols on the oxidation stability of methyl esters. J Am Oil Chem Soc 84:579–585CrossRefGoogle Scholar
  2. 2.
    Bostyn S, Duval-Onen F, Porte C, Coic J, Fauduet H (2008) Kinetic modeling of the degradation of the α-tocopherol in biodiesel-rape methyl ester. Biores Technol 99:6439–6445CrossRefGoogle Scholar
  3. 3.
    Knothe G (2007) Some aspects of biodiesel oxidative stability. Fuel Process Technol 88:669–677CrossRefGoogle Scholar
  4. 4.
    Pauls RE (2011) Fast gas chromatographic separation of biodiesel. J Chromatogr Sci 49:370–374CrossRefGoogle Scholar
  5. 5.
    Ruperez FJ, Martin D, Herrera E, Barbas C (2001) Chromatographic analysis of α-tocopherol and related compounds in various matrices. J Chromatogr A 935:45–69CrossRefGoogle Scholar
  6. 6.
    Schwartz H, Ollilainen V, Piironen V, Lampi A (2008) Tocopherol, tocotrienol and plant sterol contents of vegetable oils and industrial fats. J Food Comp Anal 21:152–161CrossRefGoogle Scholar
  7. 7.
    Nielsen MM, Hansen A (2008) Rapid high-performance liquid chromatography determination of tocopherols and tocotrienols in cereals. Cereal Chem 85:248–251CrossRefGoogle Scholar
  8. 8.
    Gruszka J, Kruk J (2007) RP-LC for determination of plastochromanol, tocotrienols and tocopherols in plant oils. Chromatographia 66:909–913CrossRefGoogle Scholar
  9. 9.
    Chauveau-Duriot B, Doreau M, Noziere P, Graulet B (2010) Simultaneous quantification of carotenoids, retinol, and tocopherols in forages, bovine plasma, and milk: validation of a novel UPLC method. Anal Bioanal Chem 397:777–790CrossRefGoogle Scholar
  10. 10.
    Citova I, Havlikova L, Urbanek L, Solichova D, Novakova L, Solich P (2007) Comparison of a novel ultra-performance liquid chromatographic method for determination of retinol and α-tocopherol in human serum with conventional HPLC using monolithic and particulate columns. Anal Bioanal Chem 388:675–681CrossRefGoogle Scholar
  11. 11.
    Snyder LR, Kirkland JJ, Dolan JW (2010) Introduction to modern liquid chromatography, 3rd edn. Wiley, New YorkGoogle Scholar
  12. 12.
    Swartz ME (2005) UPLC: an introduction and review. J Liq Chromatogr Relat Technol 28:1253–1263CrossRefGoogle Scholar
  13. 13.
    Bukovits GJ, Lezerovich A (1987) Determination of individual tocopherols by derivative spectrophotometry. J Am Oil Chem Soc 64:515–520CrossRefGoogle Scholar
  14. 14.
    Miller JC, Miller JN (1988) Statistics for analytical chemistry, 2nd edn. Wiley, New YorkGoogle Scholar
  15. 15.
    Freedman B, Kwolek WF, Pryde EH (1986) Quantitation in the analysis of transesterified soybean oil by capillary gas chromatography. J Am Oil Chem Soc 63:1370–1375CrossRefGoogle Scholar
  16. 16.
    Plank C, Lorbeer E (1995) Simultaneous determination of glycerol, and mono-, di-, and triglycerides in vegetable oil methyl esters by capillary gas chromatography. J Chromatogr A 697:461–468Google Scholar
  17. 17.
    Pauls RE (2011) A review of chromatographic characterization techniques for biodiesel and biodiesel blends. J Chromatogr Sci 49:384–396CrossRefGoogle Scholar
  18. 18.
    Gunstone FD, Harwood JL, Padley FB (1994) The lipid handbook. Chapman & Hall, LondonGoogle Scholar
  19. 19.
    Dunn RO (2005) Effect of antioxidants on the oxidative stability of methyl soyate (biodiesel). Fuel Process Technol 86:1071–1085CrossRefGoogle Scholar
  20. 20.
    Mittelbach M, Schober S (2003) The influence of antioxidants on the oxidative stability of biodiesel. J Am Oil Chem Soc 80:817–823CrossRefGoogle Scholar
  21. 21.
    Guzman R, Tang H, Salley S, Ng KYS (2009) Synergistic effects of antioxidants on the oxidative stability of soybean oil- and poultry fat-based biodiesel. J Am Oil Chem Soc 86:459–467CrossRefGoogle Scholar

Copyright information

© AOCS 2012

Authors and Affiliations

  1. 1.Chemical Sciences and Engineering DivisionArgonne National LaboratoryArgonneUSA

Personalised recommendations