Skip to main content
Log in

Determination of Nutritional and Cyclopropenoid Fatty Acids in Cottonseed by a Single GC Analysis

  • Original Paper
  • Published:
Journal of the American Oil Chemists' Society

Abstract

Historically, a complete analysis of cottonseed fatty acids required two separate analyses: gas chromatography (GC) for nutritional fatty acids and a separate analysis for cyclopropenoid fatty acids (CPFA). Using base esterification and optimized GC conditions, the method presented combines both analyses into a single GC procedure that improves analytical processes and streamlines workflow. While there were challenges, the resolution of critical pairs malvalic/stearic and dihydrosterculic/alpha linolenic methyl esters were adequately separated, allowing for accurate quantitation. Single lab reproducibility measurements (RSD) for major nutritional fatty acids ranged from 0.7 to 2.0 %. For CPFA the RSD ranged from 1.1 to 5.4 %, with the higher variability seen in the extracted cottonseed. In oils, the precision was similar between nutritional fatty acids and CPFA at equivalent concentrations, indicating the variation comes from the extraction process. Average spiked recovery results ranged from 93.3 to 106.5 % for selected fatty acids. In addition, complete fatty acid profile results compare favorably with other methodologies and historical data, demonstrating that it is possible to combine two legacy methods into one.

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

Access this article

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

Instant access to the full article PDF.

Fig. 1
Fig. 2
Fig. 3

Similar content being viewed by others

References

  1. The Organization for Economic Co-operation and Development (2009) Consensus document on compositional considerations for new varieties of cotton (Gossypium hirsutum and Gossypium barbadense): key food and feed nutrients and anti-nutrients. http://www.oecd.org/env/ehs/biotrack/46815236.pdf. Accessed 1 Sept 2014

  2. Halphen G (1897) Réaction caractéristique de l’huile de coton. J Pharm Chim 6:390–392

    CAS  Google Scholar 

  3. Harris JA, Magne FC, Skau EL (1964) Methods for the determination of cyclopropenoid fatty acids. IV. Application of the step-wise HBr titration method to the analysis of refined and crude cottonseed oils. J Am Oil Chem Soc 41:309–311

    Article  CAS  Google Scholar 

  4. Deutschman AJ, Klaus IS (1960) Spectrophotometric determination of sterculic acid. Anal Chem 32:1809–1810

    Article  CAS  Google Scholar 

  5. Obert JC, Hughes D, Sorenson WR, McCann M, Ridley WP (2007) A quantitative method for the determination of cyclopropenoid fatty acids in cottonseed, cottonseed meal, and cottonseed oil (Gossypium hirsutum) by high-performance liquid chromatography. J Agric Food Chem 55:2062–2067

    Article  CAS  Google Scholar 

  6. Wood R (1986) High performance liquid chromatography analysis of cyclopropene fatty acids. Biochem Arch 2:63–71

    CAS  Google Scholar 

  7. Park SW, Rhee K (1988) A capillary GC determination of cyclopropenoid fatty acids in cottonseed oils. J Food Sci 53:1497–1502

    Article  CAS  Google Scholar 

  8. Christie WW (1989) Gas chromatography and lipids. P.J. Barnes and Associates (Oily Press Ltd.), Dundee

  9. Dowd MK, Farve MC (2013) Fatty acid composition of Tilia spp. seed oils. Grasas Y Aceites 64:243–249

    Article  CAS  Google Scholar 

  10. Dowd MK, Boykin DL, Meredith WR Jr, Campbell BT, Bourland FM, Gannaway JR, Glass KM, Zhang J (2010) Fatty acid profiles of cottonseed genotypes from the national cotton variety trials. J Cotton Sci 14:64–73

    CAS  Google Scholar 

  11. AOAC (2012) Official methods of analysis of AOAC INTERNATIONAL, 19th Ed Method 948.22, AOAC International, Gaithersburg

  12. United States Pharmacopeia, USP37-NF32 (2014) Chromatography <621>

  13. AOCS (2013) Official methods and recommended practices of the American oil chemists’ society, 6th edn. Official Method Ce 2-66. AOCS Press, Champaign

  14. United States Pharmacopeia, USP37-NF32 (2014) Fixed fats and oils <401>, acid value

  15. Fisher GS, Cherry JP (1983) Variation of cyclopropenoid fatty acids in cottonseed lipids. Lipids 18:589–594

    Article  CAS  Google Scholar 

  16. Dowd MK (2012) Identification of the unsaturated heptadecyl fatty acids in the seed oils of Thespesia populnea and Gossypium hirsutum. JAOCS 89:1599–1609

    CAS  Google Scholar 

  17. The AOCS Lipid Library (2014) Methyl esters of fatty acids—archive of mass spectra. http://lipidlibrary.aocs.org/ms/arch_me/index.htm

  18. Aued-Pimentel S, Lago JHG, Chaves MH, Kumagai EE (2004) Evaluation of a methylation procedure to determine cyclopropenoids fatty acids from Sterculia striata St. Hil. Et Nauds seed oil. J Chromatogr A 1054:235–239

    Article  CAS  Google Scholar 

  19. AOCS (2013) Official methods and recommended practices of the American Oil Chemists’ Society, 6th edn. Official Method Ce 1i-07. AOCS Press, Champaign

  20. International Conference on Harmonisation (2005) ICH harmonized tripartite guideline, validation of analytical procedures: text and methodology Q2(R1). http://www.ich.org/fileadmin/Public_Web_Site/ICH_Products/Guidelines/Quality/Q2_R1/Step4/Q2_R1__Guideline.pdf. Accessed 28 Oct 2014

  21. International Life Sciences Institute (2014) Crop composition database, version 4.2. https://www.cropcomposition.org/query/index.html. Accessed on Apr 2014

  22. Wan PJ, Pakarinen DR, Wakelyn PJ (1998) Concerns for the determination of free fatty acid in cottonseed. J Am Oil Chem Soc 75:1321–1324

    Article  CAS  Google Scholar 

Download references

Acknowledgments

The authors would like to thank Holly Baganz, Andy Dyer, David Ellingson, Sharon Habeck, Stephanie Jolitz, Sarah Kanable, Danielle Michalica, Chris Richard, and Matt Yerges.

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Barb Mitchell.

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Mitchell, B., Rozema, B., Vennard, T. et al. Determination of Nutritional and Cyclopropenoid Fatty Acids in Cottonseed by a Single GC Analysis. J Am Oil Chem Soc 92, 947–956 (2015). https://doi.org/10.1007/s11746-015-2669-5

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s11746-015-2669-5

Keywords

Navigation