Marine oils are commonly added to conventional foods and dietary supplements to enhance their contents of omega-3 polyunsaturated fatty acids (PUFA), including eicosapentaenoic acid (EPA; 20:5n-3) and docosahexaenoic acid (DHA; 22:6n-3), which have been associated with numerous potential health benefits. This study compared American Oil Chemists' Society (AOCS) Official Methods Ce 2b-11 and Ce 2c-11 for determining EPA and DHA in foods and dietary supplements and found that AOCS Ce 2c-11 produces significantly higher analyzed values, which could be attributed to a more comprehensive breakdown of the sample matrix and derivatization of fatty acids. Our subsequent food matrix extension validation of AOCS Ce 2c-11 demonstrated that the method produces true, accurate, sensitive, and precise determinations of EPA, DHA, and total omega-3 PUFA in foods and dietary supplements containing added marine oil, including those formulated with emulsified and microencapsulated oils. The method detection limits for EPA and DHA were 0.012 AE 0.002 and 0.011 AE 0.003 mg g −1 , respectively (means AE SD). The analyzed contents of EPA (1.26-386 mg serving −1 ), DHA (1.37-563 mg serving −1 ), and total omega-3 PUFA (2.69-1270 mg serving −1 ) were reported for 27 conventional food and dietary supplement products. Eighteen products declared contents of DHA, EPA + DHA, or total omega-3 PUFA on product labels, and the analyzed contents of those fatty acids varied from 95 to 162% of label declarations for all but two of the products.Keywords Lipid analysis Á Marine oil Á Method validation Á Microencapsulation Á Omega-3 polyunsaturated fatty acids J Am Oil Chem Soc (2019) 96: 509-522.

No abstract

The United States Food and Drug Administration (FDA) recently issued its final determination that partially hydrogenated oils (PHO) are no longer generally recognized as safe (GRAS) for any use in human food. Consequently, the discrimination between PHO and fully hydrogenated oils (FHO), which is achieved by the iodine value (IV), has become an important regulatory issue. This study compared American Oil Chemists' Society (AOCS) and International Organization for Standardization (ISO) titration and gas chromatography with flame-ionization detection (GC-FID) methodologies for the determination of IV in seven samples of hydrogenated oil, namely coconut, cottonseed (n = 2), palm kernel, palm stearine, and soybean (n = 2) oils. Titrations produced statistically higher IV determinations than those achieved by GC-FID, for all samples except the FH coconut oil. The unsaponifiable matter content of the hydrogenated oils, which varied from 0.15% to 0.47% of total fat, likely contributed modest increases to the IV by titration. Both methodologies were prone to issues at low IV (~4), with titrations showing greater variability, and GC-FID being susceptible to incomplete separation, identification, and quantification of all unsaturated fatty acids. The variability observed with titrations could be minimized by careful execution of the titration protocol. Although both approaches successfully discriminated PHO and FHO in the test materials, at low IV (~4), titration is the most accurate method for determining the IV, and the only approach that has been validated in oils with a very low IV (<1).