Skip to main content
SpringerLink
Log in

Gas chromatographic quantification of fatty acid methyl esters: Flame ionization detection vs. Electron impact mass spectrometry

  • Methods
  • Published:
Lipids

Abstract

The determination of FAME by GC is among the most commonplace analyses in lipid research. Quantification of FAME by GC with FID has been effectively performed for some time, whereas detection with MS has been used chiefly for qualitative analysis of FAME. Nonetheless, the sensitivity and selectivity of MS methods advocate a quantitative role for GC-MS in FAME analysis—an approach that would be particularly advantageous for FAME determination in complex biological samples, where spectrometric confirmation of analytes is advisable. To assess the utility of GC-MS methods for FAME quantification, a comparative study of GC-FID and GC-MS methods has been conducted. FAME in prepared solutions as well as a biological standard reference material were analyzed by GC-FID and GC-MS methods using both ion trap and quadrupole MS systems. Quantification by MS, based on total ion counts and processing of selected ions, was investigated for FAME ionized by electron impact. Instrument precision, detection limits, calibration behavior, and response factors were investigated for each approach, and quantitative results obtained by each technique were compared. Although there were a number of characteristic differences between the MS methods and FID with respect to FAME analysis, the quantitative performance of GC-MS compared satisfactorily with that of GC-FID. The capacity to combine spectrometric examination and quantitative determination advances GC-MS as a powerful alternative to GC-FID for FAME analysis.

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

Similar content being viewed by others

Abbreviations

AR:

area ratio

EI:

electron impact

IT:

ion trap

LOD:

limit of detection

QP:

quadrupole

RF:

response factor

RSD:

relative SD

SIE:

selected ion extraction

SIM:

selective ion monitoring

SRM:

Standard Reference Material

TIC:

total ion counts

References

  1. James, A.T., and Martin, A.J.P. (1952) Gas-Liquid Partition Chromatography: The Separation and Micro-estimation of Volatile Fatty Acids from Formic Acid to Dodecanoic Acid, Biochem. J. 50, 679–690.

    PubMed  CAS  Google Scholar 

  2. Cropper, F.R., and Heywood, A. (1953) Analytical Separation of the Methyl Esters of the C12−C22 Fatty Acids by Vapour-Phase Chromatography, Nature 172, 1101–1102.

    Article  CAS  Google Scholar 

  3. Ackman, R.G. (1990) Misidentification of Fatty Acid Methyl Ester Peaks in Liquid Canola Shortening, J. Am. Oil Chem. Soc. 67, 1028.

    CAS  Google Scholar 

  4. Hawrysh, Z.J., Shand, P.J., Lin, C., Tokarska, B., and Hardin, R.T. (1990) Efficacy of Tertiary Butylhydroquinone on the Storage and Heat Stability of Liquid Canola Shortening, J. Am. Oil Chem. Soc. 67, 585–590.

    CAS  Google Scholar 

  5. Johnson, A.R., Fogerty, A.C., Hood, R.L., Kozuharov, S., and Ford, G.L. (1976) Gas-Liquid Chromatography of Ethyl Ester Artifacts Formed During the Preparation of Fatty Acid Methyl Esters, J. Lipid Res. 17, 431–432.

    PubMed  CAS  Google Scholar 

  6. David, F., Sandra, P., and Wylie, P.L. (2002) Improving Analysis of Fatty Acid Methyl Esters Using Retention Time Locked Methods and Retention Time Databases, Agilent Technologies Application Note 5988-5871EN, Palo Alto, CA.

  7. Torres, A.G., Trugo, N.M.F., and Trugo, L.C. (2002) Mathematical Method for the Prediction of Retention Times of Fatty Acid Methyl Esters in Temperature-Programmed Capillary Gas Chromatography, J. Agric. Food Chem. 50, 4156–4163.

    Article  PubMed  CAS  Google Scholar 

  8. Majos, S.A. (2003) Identification of Fatty Acids in Gas Chromatography by Application of Different Temperature Programs on a Single Capillary Column, J. Chromatogr. A 1015, 151–161.

    Article  Google Scholar 

  9. Eder, K. (1995) Gas Chroamtographic Analysis of Fatty Acid Methyl Esters, J. Chromatogr. B 671, 113–131.

    CAS  Google Scholar 

  10. Roach, J.A.G., Yurawecz, M.P., Kramer, J.K.G., Mossoba, M.M., Eulitz, K., and Ku, Y. (2000) Gas Chromatography-High Resolution Selected-Ion Mass Spectrometric Identification of Trace 21∶0 and 20∶2 Fatty Acids Eluting with Conjugated Linoleic Acid Isomers, Lipids 35, 797–802.

    Article  PubMed  CAS  Google Scholar 

  11. Janssen, G., and Parmentier, G. (1978) Determination of Double Bond Positions in Fatty Acids with Conjugated Double Bonds, Biomed. Mass Spectrom. 5, 439–443.

    Article  PubMed  CAS  Google Scholar 

  12. Christie, W.W., Brechany, E.Y., Johnson, S.B., and Holman, R.T. (1986) A Comparison of Pyrrolidide and Picolinyl Ester Derivatives for the Identification of Fatty Acids in Natural Samples by Gas Chromatography-Mass Spectrometry, Lipids 21, 657–661.

    PubMed  CAS  Google Scholar 

  13. Christie, W.W., Brechany, E.Y., and Holman, R.T. (1987) Mass Spectra of the Picolinyl Esters of Isomeric Mono- and Dienoic Fatty Acids, Lipids 22, 224–228.

    PubMed  CAS  Google Scholar 

  14. Harvey, D.J. (1998) Picolinyl Esters for the Structural Determination of Fatty Acids by GC/MS, Mol. Biotechnol. 10, 251–260.

    PubMed  CAS  Google Scholar 

  15. Christie, W.W. (1998) Gas Chroamtography-Mass Spectrometry Methods for Structural Analysis of Fatty Acids, Lipids 33, 343–353.

    Article  PubMed  CAS  Google Scholar 

  16. Choi, M.H., and Chung, B.C. (2000) Diagnostic Fragmentation of Saturated and Unsaturated Fatty Acids by Gas Chromatography-Mass Spectrometry with Pentafluorophenyldimethylsilyl Derivatization, Anal. Biochem. 277, 271–273.

    Article  PubMed  CAS  Google Scholar 

  17. Hamilton, J.T., and Christie, W.W. (2000) Mechanisms for Ion Foration During the Electron Impact-Mass Spectrometry of Picolinyl Ester and 4,4-Dimethyloxazoline Derivatives of Fatty Acids, Chem. Phys. Lipids 105, 93–104.

    Article  PubMed  CAS  Google Scholar 

  18. Koza, T., Rezanka, T., and Wurst, M. (1989) Quantitative Analysis of Fatty Acid Methyl Esters by Capillary Gas Chromatography with Flame-Ionization Detection: Quadrupole and Sector Mass Spectrometer, Folia Microbiol. 34, 165–169.

    CAS  Google Scholar 

  19. May, W.E., and Rumble, J. (2002) Certificate of Analysis, Standard Reference Material 1946, Lake Superior Fish Tissue, National Institute of Standards and Technology, Gaithersburg, MD.

    Google Scholar 

  20. Richter, B.E., Jones, B.A., Ezzell, J.L., Porter, N.L., Avdalovic, N., and Pohl, C. (1996) Accelerated Solvent Extraction: A Technique for Sample Preparation, Anal. Chem. 68, 1033–1039.

    Article  CAS  Google Scholar 

  21. Schafer, K. (1998) Accelerated Solvent Extraction of Lipids for Determining the Fatty Acid Composition of Biological Material, Anal. Chim. Acta 358, 69–77.

    Article  CAS  Google Scholar 

  22. Boselli, E., Velazco, V., Caboni, M.F., and Lercker, G. (2001) Pressurized Liquid Extraction of Lipids for the Determination of Oxysterols in Egg-Containing Food, J. Chromatogr. A 917, 239–244.

    Article  PubMed  CAS  Google Scholar 

  23. Richardson, R.K. (2001) Determination of Fat in Dairy Products Using Pressurized Solvent Extraction, J. Assoc. Off. Anal. Chem. Int. 84, 1522–1533.

    CAS  Google Scholar 

  24. Moreau, R.A., Powell, M.J., and Singh, V. (2003) Pressurized Liquid Extraction of Polar and Nonpolar Lipids in Corn and Oats with Hexane, Methylene Chloride, Isopropanol, and Ethanol, J. Am. Oil Chem. Soc. 80, 1063–1067.

    CAS  Google Scholar 

  25. Toschi, T.G., Bendini, A., Ricci, A., and Lercker, G. (2003) Pressurized Solvent Extraction of Total Lipids in Poultry Meat, Food Chem. 83, 551–555.

    Article  CAS  Google Scholar 

  26. Zhuang, W., McKague, B., Reeve, D., and Carrey, J. (2004) A Comparative Evaluation of Accelerated Solvent Extraction and Polytron Extraction for Quantification of Lipids and Extractable Organochlorine in Fish, Chemosphere 54, 467–480.

    Article  PubMed  CAS  Google Scholar 

  27. Dodds, E.D., McCoy, M.R., Geldenhuys, A., Rea, L.D., and Kennish, J.M. (2004) Microscale Recovery of Total Lipids from Fish Tissue by Accelerated Solvent Extraction, J. Am. Oil Chem. Soc. 81, 835–840.

    CAS  Google Scholar 

  28. Miller, J.N., and Miller, J.C. (2000) Statistics and Chemometrics for Analytical Chemistry, 4th edn., pp. 120–123, Pearson Education, Essex.

    Google Scholar 

  29. Ackman, R.G. (2002) The Gas Chromatograph in Practical Analyses of Common and Uncommon Fatty Acids for the 21st Century, Anal. Chim. Acta 465, 175–192.

    Article  CAS  Google Scholar 

  30. Ulberth, F., Gabernig, R.G., and Schrammel, F. (1999) Flame-Ionization Detector Response to Methyl, Ethyl, Propyl, and Butyl Esters of Fatty Acids, J. Am. Oil Chem. Soc. 76, 263–266.

    CAS  Google Scholar 

  31. Ackman, R.G., and Sipos, J.C. (1964) Application of Specific Response Factors in the Gas Chromatographic Analysis of Methyl Esters of Fatty Acids with Flame Ionization Detectors, J. Am. Oil Chem. Soc. 41, 377–378.

    CAS  Google Scholar 

  32. Craske, J.D., and Bannon, C.D. (1987) Gas Liquid Chromatography Analysis of the Fatty Acid Composition of Fats and Oils: A Total System for High Accuracy, J. Am. Oil Chem. Soc. 64, 1413–1417.

    CAS  Google Scholar 

  33. Horman, I., and Traitler, H. (1989) Routine Gas Chromatographic/Mass Spectrometric Analysis of Fatty Acid Methyl Esters Using the Ion Trap Detector, Biomed. Environ. Mass Spectrom. 18, 1016–1022.

    Article  PubMed  CAS  Google Scholar 

  34. Seppanen-Laakso, T., Laakso, I., and Hiltunen, R. (2002) Analysis of Fatty Acids by Gas Chromatography, and Its Relevance to Research on Health and Nutrition, Anal. Chim. Acta 465, 39–62.

    Article  CAS  Google Scholar 

Download references

Author information

Author notes

  1. Eric D. Dodds

    Present address: Department of Chemistry, University of California Davis, One Shields Ave., 95616, Davis, CA

Authors and Affiliations

  1. Applied Science, Engineering, and Technology Laboratory, University of Alaska Anchorage, 99508, Anchorage, Alaska

    Eric D. Dodds, Mark R. McCoy & John M. Kennish

  2. Environment and Natural Resources Institute, University of Alaska Anchorage, 99501, Anchorage, Alaska

    Lorrie D. Rea

  3. Alaska Department of Fish and Game, Physiological Ecology Laboratory, 99518, Anchorage, Alaska

    Mark R. McCoy & Lorrie D. Rea

  4. Department of Chemistry, University of Alaska Anchorage, 3211 Providence Dr., 99508, Anchorage, AK

    John M. Kennish

Authors
  1. Eric D. Dodds
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Mark R. McCoy
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Lorrie D. Rea
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. John M. Kennish
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to John M. Kennish.

About this article

Cite this article

Dodds, E.D., McCoy, M.R., Rea, L.D. et al. Gas chromatographic quantification of fatty acid methyl esters: Flame ionization detection vs. Electron impact mass spectrometry. Lipids 40, 419–428 (2005). https://doi.org/10.1007/s11745-006-1399-8

Download citation

  • Received:

  • Accepted:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s11745-006-1399-8

Keywords

Search

Navigation