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Determination of Docosahexaenoic Acid and n-3 Fatty Acids in Refined Fish Oils by H-NMR Spectroscopy: IUPAC Interlaboratory Study

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A high-resolution proton nuclear magnetic resonance (NMR) method for determining the concentration (mg/g) of docosahexaenoic acid (DHA), the molar proportion (mol%) of DHA, and the molar proportion of total n-3 fatty acids in fish oils was validated by an IUPAC interlaboratory study (the Commission VI-6 on Oils, Fats, and Derivatives WG 3/98). Thirteen laboratories from 5 countries tested 6 pairs of blind duplicate fish oils: a refined tuna oil, 2 extracted tuna oils, an extracted bonito oil, an extracted salmon oil, and an extracted sardine oil ranging from 9 to 30 mol% DHA and from 20 to 35 mol% n-3 fatty acids. Before 1D-proton NMR measurements with 300–500 MHz instruments, oil samples were weighed and diluted with deuterochloroform solution containing ethylene glycol dimethyl ether as internal standard. To achieve precise performance, a detailed procedure for signal area measurement was described in the protocol, and all participants were instructed about the critical importance of following the protocol. Statistical performances with invalid and outlier data removed were as follows: repeatability relative standard deviations (RSDr) ranged from 0.91 to 2.62% and reproducibility relative standard deviation (RSDR) ranged from 1.73 to 4.27% for DHA concentration (mg/g); RSDr ranged from 0.39 to 2.06%, and RSDR ranged from 0.59 to 3.46% for mol% DHA; RSDr ranged from 0.23 to 0.90% and RSDR ranged from 0.85 to 2.01% for mol% total n-3 fatty acids. The method is expected to be recommended by IUPAC.
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Document Type: Research Article

Affiliations: 1: Japan Marine Oil Association, 32-7 Motoyoyogi-cho, Shibuya-ku, 151-0062, Tokyo, Japan; Japan Food Research Laboratories, Tama Laboratory, 6-11-10 Nagayama, Tama-shi, 206-0025, Tokyo, Japan. 2: SINTEF, Division of Applied Chemistry, Fisheries and Aquaculture, N-7034, Trondheim, Norway. 3: University of Naples Federico II, Department of Food Science, Parco Gussone, 80055 Portici, Italy. 4: University of Naples Federico II, Department of Chemistry, via Mezzocannone 4, 80134 Naples, Italy. 5: Japan Marine Oil Association, 32-7 Motoyoyogi-cho, Shibuya-ku, 151-0062, Tokyo, Japan. 6: Tokyo University of Fisheries, Department of Food Science and Technology, 4-5-7 Konan, Minato-ku, 108-8477, Tokyo, Japan.

Publication date: 2002-11-01

More about this publication?
  • The Journal of AOAC INTERNATIONAL publishes refereed papers and reviews in the fields of chemical, biological and toxicological analytical chemistry for the purpose of showcasing the most precise, accurate and sensitive methods for analysis of foods, food additives, supplements and contaminants, cosmetics, drugs, toxins, hazardous substances, pesticides, feeds, fertilizers and the environment available at that point in time. The scope of the Journal includes unpublished original research describing new analytical methods, techniques and applications; improved approaches to sampling, both in the field and the laboratory; better methods of preparing samples for analysis; collaborative studies substantiating the performance of a given method; statistical techniques for evaluating data. The Journal will also publish other articles of general interest to its audience, e.g., technical communications; cautionary notes; comments on techniques, apparatus, and reagents.
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