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Journal of Lipid Research, Vol. 44, 2406-2427, December 2003
Copyright © 2003 by American Society for Biochemistry and Molecular Biology

Methods

Multicomponent analysis of encapsulated marine oil supplements using high-resolution ¹H and ¹³C NMR techniques

Navaede Siddiqui^*, Julia Sim^*, Christopher J. L. Silwood^*, Harold Toms, Richard A. Iles^* and Martin Grootveld^1,

^* Department of Diabetes and Metabolic Medicine, Barts and the London, Queen Mary's School of Medicine and Dentistry, Whitechapel, London E1 1BB, United Kingdom
Department of Chemistry, Queen Mary University of London, Mile End Road, London E1 4NS, United Kingdom
School of Dentistry, The Queen's University of Belfast, Royal Victoria Hospital, Grosvenor Road, Belfast BT12 6BP, Northern Ireland

¹ To whom correspondence should be addressed at Room AW518, Medical Unit, 5th Floor, Alexandra Wing, Royal London Hospital, London E1 1BB, United Kingdom. e-mail: m.grootveld{at}qmul.ac.uk

Multicomponent high-resolution ¹H and ¹³C NMR analysis has been employed for the purpose of detecting and quantifying a wide range of fatty acids (as triacylglycerols or otherwise) in encapsulated marine cod liver oil supplements. The ¹H NMR technique provided quantitative data regarding the docosahexaenoic acid content of these products, which serves as a valuable index of fish oil quality, and a combination of both ¹H and ¹³C spectroscopies permitted the analysis of many further components therein, including sn-1 monoacylglycerols, sn-1,2 and -1,3 diacylglycerol adducts, together with a range of minor components, such as trans-fatty acids, free glycerol and cholesterol, and added vitamins A and E. The identities of each of the above agents were confirmed by the application of two-dimensional ¹H-¹H spectroscopies. The NMR techniques employed also uniquely permitted determinations of the content of nonacylglycerol forms of highly unsaturated (or other) fatty acids in these products (i.e., ethyl esters), and therefore served as a means of distinguishing "natural" sources of cod liver oils from those subjected to chemical modification to and/or supplementation with synthetic derivatives such as ethyl docosahexaenoate or eicosopentaenoate.

The analytical significance and putative health effects of the results acquired are discussed.

Supplementary key words docosahexaenoic acid • eicosopentaenoic acid • n-3 fatty acids • fatty acid ethyl esters • -tocopherol acetate • all-trans-retinol palmitate • regiospecific analysis

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