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.
Similar content being viewed by others
References
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
Halphen G (1897) Réaction caractéristique de l’huile de coton. J Pharm Chim 6:390–392
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
Deutschman AJ, Klaus IS (1960) Spectrophotometric determination of sterculic acid. Anal Chem 32:1809–1810
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
Wood R (1986) High performance liquid chromatography analysis of cyclopropene fatty acids. Biochem Arch 2:63–71
Park SW, Rhee K (1988) A capillary GC determination of cyclopropenoid fatty acids in cottonseed oils. J Food Sci 53:1497–1502
Christie WW (1989) Gas chromatography and lipids. P.J. Barnes and Associates (Oily Press Ltd.), Dundee
Dowd MK, Farve MC (2013) Fatty acid composition of Tilia spp. seed oils. Grasas Y Aceites 64:243–249
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
AOAC (2012) Official methods of analysis of AOAC INTERNATIONAL, 19th Ed Method 948.22, AOAC International, Gaithersburg
United States Pharmacopeia, USP37-NF32 (2014) Chromatography <621>
AOCS (2013) Official methods and recommended practices of the American oil chemists’ society, 6th edn. Official Method Ce 2-66. AOCS Press, Champaign
United States Pharmacopeia, USP37-NF32 (2014) Fixed fats and oils <401>, acid value
Fisher GS, Cherry JP (1983) Variation of cyclopropenoid fatty acids in cottonseed lipids. Lipids 18:589–594
Dowd MK (2012) Identification of the unsaturated heptadecyl fatty acids in the seed oils of Thespesia populnea and Gossypium hirsutum. JAOCS 89:1599–1609
The AOCS Lipid Library (2014) Methyl esters of fatty acids—archive of mass spectra. http://lipidlibrary.aocs.org/ms/arch_me/index.htm
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
AOCS (2013) Official methods and recommended practices of the American Oil Chemists’ Society, 6th edn. Official Method Ce 1i-07. AOCS Press, Champaign
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
International Life Sciences Institute (2014) Crop composition database, version 4.2. https://www.cropcomposition.org/query/index.html. Accessed on Apr 2014
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
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
Corresponding author
About this article
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
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s11746-015-2669-5