Evolution of reference materials for the determination of organic nutrients in food and dietary supplements—a critical review
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For over 40 years, food-matrix certified reference materials (CRMs) have been available for determination of trace element content, and a wide variety of materials are available from most producers of CRMs. However, the availability of food-matrix CRMs for organic nutrients has been more limited. The European Commission (EC) Bureau Communautaire de Référence (BCR) and the National Institute of Standards and Technology (NIST) introduced food-matrix CRMs with values assigned for vitamins and other organic nutrients such as fatty acids and carotenoids in the 1990s. The number of organic nutrients for which values were assigned has increased significantly in the past decade, and the approach and analytical methods used for assignment of the certified values have also evolved. Recently, dietary supplement-matrix CRMs such as multivitamin tablets with values assigned for vitamins and carotenoids, and fish and plant oils with values assigned for fatty acids have appeared. The development, evolution, and improvement of food- and dietary supplement-matrix CRMs for determination of vitamins, carotenoids, and fatty acids are described, with emphasis on CRMs made available in the past 10 years. Recent food and dietary supplement CRMs for the determination of organic nutrients include infant formula, multivitamin tablets, milk and egg powders, breakfast cereal, meat homogenate, blueberries, soy flour, fish and plant oils, dry cat food, and protein drink powder. Many of these food- and supplement-matrix CRMs have values assigned for over 80 organic and inorganic nutrients, toxic elements, proximates, and contaminants. The review provides a critical assessment of the challenges and evolving improvements in the production and the analytical methods used for value assignment of these CRMs. The current status and future needs for additional food- and dietary supplement-matrix CRMs for organic nutrients are also discussed.
KeywordsCertified reference materials (CRMs) Cholesterol Dietary supplements Fatty acids Nutrients Standard reference materials (SRMs) Vitamins
The authors acknowledge Zhang Qinghe of NIMC and Byungjoo Kim of KRISS for providing valuable information regarding their CRMs and Thomas Linsinger, Håkan Emteborg, and Marta Dabrio (JRC) for useful input regarding the JRC food-matrix CRMs. Katherine E. Sharpless (NIST) and Lane C. Sander (NIST) are acknowledged for their contributions in the coordination of the development of many of the NIST food- and dietary supplement-matrix SRMs. Joseph M. Betz, Director of the Analytical Methods and Reference Materials (AMRM) Program at the Office of Dietary Supplements, National Institutes of Health, is acknowledged for his guidance and leadership in the development of dietary supplement SRMs. The contributions of the numerous analysts at NIST, JRC, NIMC, and KRISS who have provided measurements used in the certification of organic nutrients in the CRMs discussed in this review are also acknowledged.
Compliance with ethical standards
Conflict of interest
The authors declare that they have no conflict of interest.
- 2.Bowen HJM (1985) Kale as a reference material. In: Biological reference materials—availability, uses, and need for validation of nutrient measurement. John Wiley & Sons, New YorkGoogle Scholar
- 5.May W, Parris R, Beck C II, Fassett J, Greenberg R, Guenther F, et al. Definition of terms and modes used at NIST for value-assignment of reference materials for chemical measurements. NIST Special Publication, vol 260–136. Gaithersburg: National Institute of Standards and Technology (NIST); 2000.Google Scholar
- 7.Hollman PCH, Boenke A, Wagstaffe PJ (1993) The certification of major components and major elements in five food reference materials. Fresenius J Anal Chem 345 (2–4):174–179. doi: https://doi.org/10.1007/bf00322583
- 9.Parr RM, Fajgelj A, Dekner R, Ruiz HV, Carvalho FP, Povinec PP (1998) IAEA analytical quality assurance programmes to meet the present and future needs of developing countries. Fresenius J Anal Chem 360 (3–4):287–290. doi: https://doi.org/10.1007/s002160050694
- 11.Ihnat M, Dabeka RW, Wolynetz MS (1993) Summary of preparation and homogeneity characterization of 10 agricultural food reference materials for elemental composition. Fresenius J Anal Chem 345 (2–4):221–223. doi: https://doi.org/10.1007/bf00322594
- 13.Ihnat M (2001) Twenty five years of reference material activity at Agriculture and Agri-Food Canada. Fresenius J Anal Chem 370 (2–3):279–285. doi: https://doi.org/10.1007/s002160100803
- 14.National Research Council Canada, Certified Reference Materials, www.nrc-cnrc.gc.ca/eng/solutions/advisory/crm_index.html, accessed 4/12/2018.
- 16.U.S. Food And Drug Administration Total Diet Study. (2014) U.S. Department of Health and Human Resources, www.fda.gov/food/FoodScienceResearch/TotalDietStudy/default.htm, accessed 07-03-2018.
- 17.U.S. Infant Formula Act (1980). Public Law 96–359 [H.R. 6940]; Sept 26, 1980, www.gpo.gov//fdsys/pkg/Statute-94/pdf/statute-94-Pg1190.pdf, accessed 07-03-2018.
- 18.U.S. Food and Drug Administration (1990) Nutrition Labeling and Education Act. Public Law 101–535 [H.R. 3562], Nov. 8 1990, www.gpo.gov/fdsys/pkg/statute-104/statute-104-Pg2353.pdf, accessed 07-03-2018.
- 19.U.S. Department Health and Human Services, Food and Drug Administration, Food Safety Moderization Act (FSMA) (2011), www.fda.gov/food/guidanceRegulation/FSMA, accessed 2/17/2018.
- 20.U.S. Dietary Supplement Health and Education Act (DSHEA) of 1994 Public Law 103–417, 103rd Congress, accessed 2/17/2018.Google Scholar
- 21.U.S. Department Health and Human Services, Food and Drug Administration, Current Good Manufacturing Practices (CGMPs) for Dietary Supplements (2007), www.fda.gov/food/guidanceRegulation/CGMP, accessed 2/17/2018.
- 22.European Commission Directive, Food (2014), www.ec.europa.eu/food/safety/labeling_nutrition/labelling_legislation_en, accessed 2/18/2018.
- 23.National Food Safety Standard - Infant Formula (2009). The Ministry of Health of the People’s Republic of China, https://gain.fas.usda.gov/Recent%20GAIN%20Publications/National%20Dairy%20Standard%20-%20Infant%20Formulas_Beijing_China%20-%20Peoples%20Republic%20of_12-1-2009.pdf, accessed on 2/18/2018.
- 24.International Standards Organization (ISO) (2015) Reference materials—selected terms and definitions. ISO Guide 30:2015, 3rd Ed.Google Scholar
- 25.Ikins W, DeVries J, Wolf WR, Oles P, Carpenter D, Fraley N, et al. A food matrix organizational system applied to collaborative studies. The Referee AOAC International. 1993;17:1–7.Google Scholar
- 26.Wolf WR. Reference materials. In: Methods of analysis for nutrition labeling. Arlington: AOAC International; 1993.Google Scholar
- 27.Wolf WR, Andrews KW (1995) A system for defining reference materials applicable to all food matrices. Fresenius J Anal Chem 352 (1–2):73–76. doi: https://doi.org/10.1007/bf00322300
- 29.Sharpless KE, Colbert JC, Greenberg RR, Schantz MM, Welch MJ (2001) Recent developments in food-matrix reference materials at NIST. Fresenius J Anal Chem 370 (2–3):275–278. doi: https://doi.org/10.1007/s002160100826
- 32.Sharpless KE, Welch MJ, Greenberg RR, Iyengar GV, Colbert JC (1998) Recent SRMs for organic and inorganic nutrients in food matrices. Fresenius J Anal Chem 360 (3–4):456–458. doi: https://doi.org/10.1007/s002160050738
- 33.Wise SA, Sharpless KE, Sander LC, May WE (2004) Standard reference materials to support US regulations for nutrients and contaminants in food and dietary supplements. Accredit Qual Assur 9 (9):543–550. doi: https://doi.org/10.1007/s00769-004-0820-3
- 35.Sharpless KE, Schiller SB, Margolis SA, Thomas JB, Iyengar GV, Colbert JC, Gills TE, Wise SA (1997) Certification of nutrients in standard reference material 1846: infant formula. J AOAC Int 80 (3):611–621.Google Scholar
- 36.Sharpless KE, Arce-Osuna M, Thomas JB, Gill LM (1999) Value assignment of retinol, retinyl palmitate, tocopherol, and carotenoid concentrations in standard reference material 2383 (baby food composite). J AOAC Int 82 (2):288–296.Google Scholar
- 37.Sharpless KE, Gill LM, Margolis SA, Wise SA, Elkins E (1999) Preparation of standard reference material 2383 (baby food composite) and use of an interlaboratory comparison exercise for value assignment of its nutrient concentrations. J AOAC Int 82 (2):276–287.Google Scholar
- 38.Sharpless KE, Thomas JB, Nelson BC, Phinney CS, Sieber JR, Wood LJ, Yen JH, Howell DW (2002) Value assignment of nutrient concentrations in standard reference material 2384 baking chocolate. J Agric Food Chem 50 (24):7069–7075. doi: https://doi.org/10.1021/fj020610d
- 41.Finglas PM, Scott KJ, Witthoft H, van den Berg H, de Froidmont-Goertz I. The certification of the mass fractions of vitamins in four reference materials: wholemeal flour (CRM 121), milk powder (CRM 421), lyophilized mixed vegetabbles (CRM 485) and lyophilized pigs liver (CRM 487). Luxembourg: Office for Official Publications of the European Communities; 1999.Google Scholar
- 42.Finglas PM, van den Berg H, de Froidmont-Goertz I. The certification of the mass fractions of vitamins in three reference materials: margarine (CRM 121), milk powder (CRM 421), and lyophilized brussels sprout powder (CRM 431). Luxembourg: Office for Official Publications of the European Communities; 1997.Google Scholar
- 43.Zeleny R, Bernreuther T, Linsinger T, Schimmel H, Sejeroe-Olsen B, Kramer GN, et al. The method-specific certification of thee cholesterol and triglyceride contents of a pure and an adulterated butter fat reference material BCR-632-A and BCR-632B. Geel: European Commission Joint Research Centre; 2005.Google Scholar
- 46.Phillips MM, Bedner M, Reitz M, Burdette CQ, Nelson MA, Yen JH, et al. Liquid chromatography with absorbance detection and with isotope-dilution mass spectrometry for determination of isoflavones in soy standard reference materials. Anal Bioanal Chem. 2017;409(4):949–60. https://doi.org/10.1007/s00216-016-9997-7.CrossRefPubMedGoogle Scholar
- 50.International Standards Organization (ISO) (2016) General requirements for the competence of reference material producers. ISO Guide 17034, 1st Ed.Google Scholar
- 56.Cohen A, Hertz HS, Mandel J, Paule RC, Schaffer R, Sniegoski LT, Sun T, Welch MJ, White E (1980) Total serum-cholesterol by isotope dilution-mass spectrometry—a candidate definitive method. Clin Chem 26 (7):854–860.Google Scholar
- 60.Nelson BC, Sharpless KE, Sander LC. Improved liquid chromatography methods for the separation and quantification of biotin in NIST standard reference material 3280: multivitamin/multielement tablets. J Agric Food Chem. 2006;54(23):8710–6. https://doi.org/10.1021/jf062000+. CrossRefPubMedGoogle Scholar
- 61.Sharpless KE, Lindstrom RM, Nelson BC, Phinney KW, Rimmer CA, Sander LC, Schantz MM, Spatz RO, Thomas JB, Turk GC, Wise SA, Wood LJ, Yen JH (2010) Preparation and characterization of standard reference material 1849 infant/adult nutritional formula. J AOAC Int 93 (4):1262–1274.Google Scholar
- 63.Certificate of Analysis, Standard Reference Materials (SRMs), National Institute of Standards and Technology (NIST) www.nist.gov/srm
- 67.Plockington WD, Pearse J, Lognay G, Wagstaffe PJ, Boenke A, Schurer B. The certification of the fatty acid profile and the cholesterol mass fraction of two edible oil and fat materials - soya-maise oil blend CRM 162, beef-pork fat blend CRM 163. Luxembourg; 1993.Google Scholar
- 70.Dabrio Ramos M, Schimmel H, Emons H. Certification of the mass fractions of vitamins in whole milk powder. Geel: Joint Research Centre, European Commission; 2011.Google Scholar
- 77.Koontz JL, Phillips KM, Wunderiach KM, Exler J, Holden JM, Gebhardt SE, et al. Comparison of total folate concentrations in foods determined by microbiological assay at several experienced US commercial laboratories. J AOAC Int. 2005;88(3):805–13.Google Scholar
- 78.U.S. Food and Drug Administration Proposed Rule 79 FR 11879 3-3-2014 (2014). www.federalregister.gov/documents/2014/0303/2014-04387/food-labeling-revision-of-the-nutrition-and-supplement-fact-labels, accessed 07-03-2018.
- 79.Taylor CL, Patterson KY, Roseland JM, Wise SA, Merkel JM, Pehrsson PR, et al. Including food 25-hydroxyvitamin D in intake estimates may reduce the discrepancy between dietary and serum measures of vitamin D status. J Nutr. 2014;144(5):654–9. https://doi.org/10.3945/jn.113.189811.CrossRefPubMedPubMedCentralGoogle Scholar
- 80.Roseland JM, Patterson KY, Andrews KW, Phillips KM, Phillips MM, Pehrsson PR, et al. Interlaboratory trial for measurement of vitamin D and 25-hydroxyvitamin D 25(OH)D in foods and a dietary supplement using liquid chromatography-mass spectrometry. J Agric Food Chem. 2016;64(16):3167–75. https://doi.org/10.1021/acs.jafc.5b05016.CrossRefPubMedPubMedCentralGoogle Scholar
- 81.Burdette CQ National Institute of Standards and Technology, Gaithersburg, MD, USA, personal communication.Google Scholar
- 84.Jing W, Thompson JJ, Jacobs WA, Salvati LM. Determination of free and total carnitine and choline in infant formulas and adult nutritional products by UPLC/MS/MS: single-laboratory validation, First Action 2014.04. J AOAC Intl. 2015;98(5):1395–406. https://doi.org/10.5740/jaoacint.12-137.CrossRefGoogle Scholar
- 85.Ellingson DJ, Shippar JJ, Gilmore JM. Determination of free and total choline and carntine in infant formula and adult/pediatric nutritional formula by liquid chromatography/tandem mass spectrometry (LC/MS/MS): Single-laboratory validation, First Action 2015.10. J. AOAC Intl. 2016;99(1):204–9. https://doi.org/10.5740/jaoacint.15102.CrossRefGoogle Scholar
- 87.European Commission, Joint Research Centre (JRC), Certified Reference Material Catalogue, https://crm.jrc.ec.europa.eu, assessed 10-25-2018.
- 88.Certificate of Analysis, Standard Reference Material 1845a Whole Egg Powder, National Institute of Standards and Technology (NIST) (2018).Google Scholar
- 89.Certificate of Analysis, Standard Reference Material (SRM) 3234 Soy Flour, National Institute of Standards and Technology (NIST) (2017).Google Scholar
- 90.U.S. Department of Agriculture, Agricultural Research Service, USDA Food Composition Databases. https://ndb.nal.usda.gov, accessed 10-25-2018.
- 93.Top 100 dietary supplements by U.S. sales 2012–2016 (2017). Nutrition Business Journal, www.nutritionbusinessjournal.com
- 94.Emteborg H, Linsinger T, European Commission Joint Research Centre, Geel, Belgium, personal communication.Google Scholar
- 95.Linsinger T. Application Note 1 Comparison of a measurement result with the certified value. Geel: European Commission - Joint Research Centre, Institute for Reference Materials and Measurements (IRMM); 2014.Google Scholar
- 96.Sharpless KE, Lippa KA, Duewer DL, Rukhin AL. Standard reference materials in the analysis of foods and dietary supplements: a practical guide. Gaithersburg: NIST Special Publication 260–181, National Institute of Standards and Technology (NIST); 2014.Google Scholar
- 98.Long SE, Catron BL, Boggs ASP, Tai SS-C, Wise SA. Development of standard reference materials to support assessment of iodine status for nutritional and public health purposes. Am J Clin Nutr. 2016;104(Supplement):902S–6S. https://doi.org/10.3945/ajcn.115.110361.CrossRefPubMedPubMedCentralGoogle Scholar