Matrix Extension Validation of AOCS Ce 2c‐11 for Omega‐3 Polyunsaturated Fatty Acids in Conventional Foods and Dietary Supplements Containing Added Marine Oil

Abstract

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.

Evaluation of Delivery Form of Eicosapentaenoic and Docosahexaenoic Acids During Quality Control of Fish Oil Supplements

“…Figure 1 shows the different profiles of FA obtained by GC-FID for a natural FO supplement (Figure 1-A, Sample 1) and a concentrated FO supplement (Figure 1-B, Sample 10). It can be observed that the natural FO presented a large number of major peaks besides EPA and DHA, with a high amount of saturated fatty acids (SFA), such as C14:0 and C16:0, monounsaturated fatty acids (MUFA), such as C16:1 and C18:1, and some characteristics PUFA, such as C16:2, C16:3, C16:4, C18:4, C21:5, and C22:5 also reported by other researchers [11,12]. Several isomers were also separated in this natural FO (C16:1, C18:1, C18:2, C18:3, 20:4, and 22:5).…”

The Importance of Reference Materials and Method Validation for Advancing Research on the Health Effects of Dietary Supplements and Other Natural Products

“…SRM 3275 has found wide use to validate methods and serve as a QC material as demonstrated by Srigley and coworkers ( 86 – 89 ) at the FDA reporting several studies using SRM 3275 for validation of methods. In a study to evaluate the overall fatty acid composition of 46 marine oil omega-3 supplements, Srigley and Rader analyzed SRM 3275 (all three levels) using GC-FID on a novel ionic liquid phase column ( 90 ).…”

The Analysis of Docosahexaenoic Acid (DHA) in Dried Dog Food Enriched with an Aurantiochytrium limacinum Biomass: Matrix Extension Validation and Verification of AOAC Method 996.06

“…Methods involving esterification are generally preferred as the resulting esters are highly volatile in the GC conditions and easy to measure ( 30 ). As government agencies and regulatory authorities often require that laboratories or researchers use AOAC methods for regulatory studies ( 30 , 31 ), the AOAC 996.06 method had previously been selected by the present authors to validate methodologies for the analysis of DHA and fatty acids in the Thraustochytrid feed ingredient, unextracted Aurantiochytrium limacinum biomass ( 32 ), which is rich in DHA and also to the analysis of edible chicken tissues enriched with DHA ( 33 ). Therefore, the current study aimed, for the first time, at validating the AOAC 996.06 method to accurately quantify DHA in dog food when enriched with an unextracted A. limacinum biomass as a matrix extension, and then to verify these results in a second laboratory.…”