Skip to main content

Rapid FT-NIR Analysis of Edible Oils for Total SFA, MUFA, PUFA, and Trans FA with Comparison to GC

Abstract

Declarations of the total content of trans fatty acids (FA) and saturated FA (SFA) are mandatory on food labels in the US and Canada. Gas chromatography (GC) has been the method of choice for the determination of FA composition. However, GC is time consuming and requires conversion of fats and oils to their FA methyl esters. In the present study, a recently published Fourier transform near-infrared (FT-NIR) spectroscopic procedure was applied to the rapid (<5 min) determination of total SFA, monounsaturated FA (MUFA), polyunsaturated FA (PUFA), and trans FA contents of 30 commercially available edible fats and oils. Good agreement was obtained between the GC and FT-NIR methods for the determination of total SFA, MUFA, and PUFA contents. Differences between the two methods were apparent for the determination of trans fat at trans fat levels <2 % of total fat. The analytical determinations of total SFA, MUFA, and PUFA contents for many of the oils examined differed from the respective values declared on the product labels. Our findings demonstrate that the FT-NIR procedure serves as a suitable alternative method for the rapid determination of total SFA, MUFA, PUFA and trans FA contents of neat vegetable oils.

This is a preview of subscription content, access via your institution.

Fig. 1
Fig. 2
Fig. 3
Fig. 4

Abbreviations

AOCS:

American Oil Chemist’s Society

ATR-FTIR:

Attenuated total reflection–Fourier transform mid-infrared

CACI-MS/MS:

Covalent adduct chemical ionization tandem mass spectrometry

CLA:

Conjugated linoleic acid

EI-MS:

Electron impact MS

FA:

Fatty acid

FAME:

FA methyl ester

FT-NIR:

Fourier transform near-infrared

GC:

Gas chromatography

MUFA:

Monounsaturated FA

PUFA:

Polyunsaturated FA

SFA:

Saturated FA

References

  1. 1.

    Department of Health and Human Services, Food and Drug Administration (2003) Food Labeling: trans fatty acids in nutrition labeling: nutrient content claims, and health claims. final rule, July 11, 2003. Fed Regist 68:41434–41506

    Google Scholar 

  2. 2.

    Department of Health (2003) Regulations amending the food and drug regulations (nutritional labelling, nutrient content claims and health claims), Canada Gazette, Part II (Ottawa, Canada) 137:154–409

  3. 3.

    AOAC Official Method 996.06 (2001) Fat (total, saturated, and unsaturated) in foods

  4. 4.

    AOCS Official Method Ce 1h-05 (2009) Determination of cis-, trans-, saturated, monounsaturated and polyunsaturated fatty acids in vegetable or non-ruminant animal oils and fats by capillary GLC. Approved 2005. In Official Methods and Recommended Practices of the AOCS, 6th Ed., AOCS, Ed. Champaign, IL

  5. 5.

    AOCS Official Method Ce 1j-07 (2009) Determination of cis-, trans-, saturated, monounsaturated and polyunsaturated fatty acids in extracted fats by capillary GLC. Re-approved 2012. In Official Methods and Recommended Practices of the AOCS, 6th Ed., AOCS, Ed. Champaign, IL

  6. 6.

    Mossoba MM, Kramer JKG (2009) Official methods for the determination of Trans fat, 2nd edn. AOCS, Urbana

    Google Scholar 

  7. 7.

    Mossoba MM, Moss J, Kramer JKG (2009) Trans fat labeling and levels in US foods: assessment of gas chromatographic and infrared spectroscopic techniques for regulatory compliance. J AOAC Internat 92:1284–1300

    CAS  Google Scholar 

  8. 8.

    Delmonte P, Fardin Kia A-R, Kramer JKG, Mossoba MM, Sidisky L, Rader JI (2011) Separation characteristics of fatty acid methyl esters using SLB-IL111, a new ionic liquid coated capillary gas chromatographic column. J Chromatogr A 1218:545–554

    Article  CAS  Google Scholar 

  9. 9.

    Kramer JKG, Hernandez M, Cruz-Hernandez C, Kraft J, Dugan MER (2008) Combining results of two GC separations partly achieves determination of all cis and trans 16:1, 18:1, 18:2, 18:3 and CLA isomers of milk fat as demonstrated using Ag-ion SPE fractionation. Lipids 43:259–273

    Article  CAS  Google Scholar 

  10. 10.

    AOCS Official Method Cd 14d-99 (2009) Rapid determination of isolated trans geometric isomers in fats and oils by attenuated total reflection infrared spectroscopy (1999). In Official Methods and Recommended Practices of the AOCS, 6th Ed., AOCS, Ed. Champaign, IL

  11. 11.

    AOAC Official Method 2000.10 (2000) Determination of total isolated trans unsaturated fatty acids in fats and oils. ATR-FTIR spectroscopy

  12. 12.

    AOCS Official Method Cd 14e-09 (2009) Negative second derivative infrared spectroscopic method for the rapid (5 min) determination of total isolated trans fat (2009). In Official Methods and Recommended Practices of the AOCS, 6th Ed., AOCS, Ed. Champaign, IL

  13. 13.

    Azizian H, Kramer JKG (2005) A rapid method for the quantification of fatty acids in fats and oils with emphasis on trans fatty acids using Fourier Transform near infrared spectroscopy (FT-NIR). Lipids 40:855–867

    Article  CAS  Google Scholar 

  14. 14.

    Azizian H, Kramer JKG, Winsborough SL (2007) Factors influencing the fatty acid determination in fats and oils using Fourier transform near-infrared spectroscopy. Eur J Lipid Sci Technol 109:960–968

    Article  CAS  Google Scholar 

  15. 15.

    Azizian H, Kramer JKG, Mossoba MM (2010) Progression of fatty acid profiling of edible fats and oils using vibrational spectroscopy. In: Li-Chan ECY, Griffiths PR, Chalmers JM (eds) Applications of vibrational spectroscopy in food science, vol II., Analysis of Food Drink and Related MaterialsWiley, Chichester, pp 519–537

    Google Scholar 

  16. 16.

    Azizian H, Kramer JKG, Mossoba MM (2012) Evaluating the transferability of FT-NIR calibration models for fatty acid determination of edible fats and oils among five same-make spectrometers using transmission or transflection modes with different pathlengths. J Am Oil Chem Soc 89:2143–2154

    Article  CAS  Google Scholar 

  17. 17.

    Tyburczy C, Mossoba MM, Fardin Kia A-R, Rader JI (2012) Evaluation of low trans fat edible oils by attenuated total reflection Fourier transform infrared spectroscopy and gas chromatography: a comparison of analytical approaches. Anal Bioanal Chem 404:809–819

    Article  CAS  Google Scholar 

  18. 18.

    Delmonte P, Hu Q, Kia AR, Rader JI (2008) Preparation, chromatographic separation and relative retention times of cis/trans heptadecaenoic (17:1) fatty acids. J Chromatogr A 1214:30–36

    Article  CAS  Google Scholar 

  19. 19.

    Delmonte P, Kia A-R, Hu Q, Rader JI (2009) Review of methods for preparation and gas chromatographic separation of trans and cis reference fatty acids. J AOAC Internat 92:1310–1326

    CAS  Google Scholar 

  20. 20.

    AOCS Official Method Ce 2-66 (2009) Preparation of methyl esters of fatty acids. In Official Methods and Recommended Practices of the AOCS, 6th Ed., AOCS, Ed. Champaign, IL

  21. 21.

    Rozema B, Mitchell B, Winters D, Kohn A, Sullivan D, Meinholz E (2008) Proposed modifications to AOAC 996.06, optimizing the determination of trans fatty acids: presentation of data. J AOAC Internat 91:92–97

    CAS  Google Scholar 

  22. 22.

    Ratnayake WM (2004) Overview of methods for the determination of trans fatty acids by gas chromatography, silver-ion thin-layer chromatography, silver-ion liquid chromatography, and gas chromatography/mass spectrometry. J AOAC Internat 87:523–539

    CAS  Google Scholar 

  23. 23.

    Brenna JT, Tyburczy C (2011) Identification of double bond location in fatty acid methyl esters by covalent adduct chemical ionization tandem mass spectrometry. http://lipidlibrary.aocs.org/topics/caci_ms/index.htm

  24. 24.

    Delmonte P, Fardin-Kia A-R, Kramer JKG, Mossoba MM, Sidisky L, Tyburczy C, Rader JI (2012) Evaluating the ionic liquid GC column SLB-IL111 for the determination of the fatty acids in milk fat. J Chromatogr A 1233:137–146

    Article  CAS  Google Scholar 

  25. 25.

    Bland JM, Altman DG (1986) Statistical methods for assessing agreement between two methods of clinical measurement. Lancet 32:307–310

    Article  Google Scholar 

  26. 26.

    Altman DG, Bland JM (1983) Measurement in medicine: the analysis of method comparison studies. Statistician 32:307–317

    Article  Google Scholar 

  27. 27.

    Hunter JE (2006) Dietary trans fatty acids: review of recent human studies and food industry responses. Lipids 41:967–992

    Article  CAS  Google Scholar 

  28. 28.

    Azizian H, Kramer JKG, Kamalian AR, Hernandez M, Mossoba MM, Winsborough SL (2004) Quantification of trans fatty acids in foods by GC, ATR-FTIR and FT-NIR methods. Lipid Technol 16:229–231

    CAS  Google Scholar 

  29. 29.

    Azizian H, Kramer JKG, Ehler S, Curtis JM (2010) Rapid quantitation of fish oil fatty acids and their ethyl esters by FT-NIR models. Eur J Lipid Sci Technol 112:452–462

    Article  CAS  Google Scholar 

  30. 30.

    Waterman E, Lockwood B (2007) Active components and clinical applications of olive oil. Altern Med Rev 12:331–342

    Google Scholar 

  31. 31.

    Spanova M, Daum G (2011) Squalene—biochemistry, molecular biology, process biotechnology, and applications. Eur J Lipid Sci Technol 113:1299–1320

    Article  CAS  Google Scholar 

  32. 32.

    Chee KM, Gong JX, Good Rees DM, Meydanl M, Ausman L, Johnson J, Siguel EN, Schaefer EJ (1990) Fatty acid content of marine oil capsules. Lipids 25:523–528

    Article  CAS  Google Scholar 

  33. 33.

    Koski A, Psomiadou E, Tsimidou M, Hopia A, Kefalas P, Wahala K, Heinonen M (2002) Oxidative stability and minor constituents of virgin olive oil and cold-pressed rapeseed oil Eur Food Res Technol 214:294–298

    Article  CAS  Google Scholar 

  34. 34.

    Delmonte P, Rader JI (2007) Evaluation of gas chromatographic methods for the determination of trans fat. Anal Bioanal Chem 389:77–85

    Article  CAS  Google Scholar 

  35. 35.

    Knoll JE (1985) Estimation of the limit of detection in chromatography. J Chromatogr Sci 23:422–425

    Article  CAS  Google Scholar 

  36. 36.

    Tyburczy C, Delmonte P, Fardin-Kia AR, Mossoba MM, Kramer JKG, Rader JI (2012) Profile of trans fatty acids (FAs) including trans polyunsaturated FAs in representative fast food samples. J Agric Food Chem 60:4567–4577

    Article  CAS  Google Scholar 

  37. 37.

    Matos LC, Cunha SC, Amaral JS, Pereira JA, Andrade PB, Seabra RM, Oliveira BPP (2007) Chemometric characterization of three varietal olive oils (C vs. Bobrancosa, Madural and Verdeal Transmontana) extracted from olives with different maturation indices. Food Chem 102:406–414

    Article  CAS  Google Scholar 

Download references

Author information

Affiliations

Authors

Corresponding author

Correspondence to Magdi M. Mossoba.

Additional information

M.M. Mossoba and H. Azizian contributed equally to this study.

About this article

Cite this article

Mossoba, M.M., Azizian, H., Tyburczy, C. et al. Rapid FT-NIR Analysis of Edible Oils for Total SFA, MUFA, PUFA, and Trans FA with Comparison to GC. J Am Oil Chem Soc 90, 757–770 (2013). https://doi.org/10.1007/s11746-013-2234-z

Download citation

Keywords

  • Fats and oils
  • Spectroscopy
  • Lipid Chemistry/Lipid Analysis