Reference Materials of the Synthetic Sweeteners Aspartame and Acesulfame Potassium

Synthetic sweeteners have found widespread application in the national economy, but their use has some limitations. Safe intake levels for aspartame and acesulfame potassium are established by the recommendations of the Joint FAO/WHO Expert Committee on Food Additives (JECFA). Compliance with safety requirements can be ensured by controlling the content of sweeteners in food products.

In Russia, measurements performed in accordance with GOST standards and certified methods, for which reference materials are essential. The presented research was conducted with the aim of replacing foreign reference materials with domestically produced reference materials to ensure measurement uniformity for the purpose of Russia’s technological sovereignty.

The publication contains information on the development of new types of reference materials for the composition of the synthetic sweeteners aspartame and acesulfame potassium, which are metrologically traceable to the State Primary Standard of units of mass (molar) fraction and mass (molar) concentration of organic components in liquid and solid substances and materials based on liquid and gas chromatography-mass spectrometry with isotope dilution and gravimetry GET 208–2024. Identification of the main component in the reference material was performed using high-resolution mass spectrometry. Characterization of the reference materials was carried out using the mass balance method. The content of related compound impurities was measured using high-performance liquid chromatography with a diode-array UV detector; the content of volatile organic compound impurities was measured using gas chromatography with a flame ionization detector; water content was determined by Karl Fischer coulometric titration. The content of non-volatile impurities was measured by gravimetry for aspartame and microwave plasma atomic emission spectrometry for acesulfame potassium. The homogeneity and long-term stability of the reference materials were studied.

The metrological characteristics of the new domestically produced reference materials demonstrate parity with foreign analogues: the mass fraction of the main component in the pure aspartame is (96.2 ± 0.3)%; the mass fraction of the main component in the pure acesulfame potassium is (99.98 ± 0.01)%.

1. Polyansky K. K., Rudakov O. B., Podporinova G. K., Khripushin V. V., Verzilina N. D. Natural and artificial sweeteners: properties and quality assessment. Мoscow : DeLi print; 2009. 252 p. (In Russ.).

2. Silina N. V., Mazurina N. V., Ershova E. V., Komshilova K. A. The effect of sweeteners on carbohydrate metabolism, metabolic parameters and intestinal microbiota. Obesity and Metabolism. 2024;21(1):58–67. (In Russ.). https://doi.org/10.14341/omet13020

3. Sezgin B., Arli G., Can N. Ö. Simultaneous HPLC-DAD determination of seven intense sweeteners in foodstuffs and pharmaceuticals using a core-shell particle column. Journal of Food Composition and Analysis. 2021;97:103768. https://doi.org/10.1016/j.jfca.2020.103768

4. Serdar M., Knežević Z. Determination of artificial sweeteners in beverages and special nutritional products using high performance liquid chromatography. Archives of Industrial Hygiene and Toxicology. 2011;62:169–173. https://doi.org/10.2478/10004 1254 62 2011 2084

5. Zygler A., Wasik A., Namieśnik J. Analytical methodologies for determination of artificial sweeteners in foodstuffs. TrAC Trends in Analytical Chemistry. 2009;28(9):1082–1102. https://doi.org/10.1016/j.trac.2009.06.008

6. Mikheeva A. Yu., Lopushanskaya E. M., Krylov A. I. Improvement of the State Primary Standard in the field of organic analysis GET 208. Measurement Standards. Reference Materials. 2024;20(4):5–19. (In Russ.). https://doi.org/10.20915/207711772024204 5 19

7. Mikheeva A. Yu. Measuring the purity of organic chemicals: general approaches and development of an appropriate procedure for research of pure organic chemicals. Izmeritel’naya Tekhnika. 2024;73(8):56–68. (In Russ.). https://doi.org/10.32446/0368–1025it.2024 8 56 68

8. Duewer D. L., Parris R. M., White V. E., May W. E. An approach to the metrologically sound traceable assessment of thechemical purity of organic reference materials. NIST Special Publication. 2004;1012:55.

9. Westwood S., Choteau T., Daireaux A., Josephs R. D., Wielgosz R. I. Mass balance method for the SI value assignment of the purity of organic compounds. Analytical Chemistry. 2013;85(6):3118–3126. https://doi.org/10.1021/ac303329k

10. Milman B. L., Zhurkovich I. K. Summarized criteria of chemical compounds identification by chromatography-mass spectrometry. Analitika i kontrol’ [Analytics and Control]. 2020;24(3):164–173. (In Russ.). https://doi.org/10.15826/analitika.2020.24.3.003

11. Stamp J. A., Labuza T. P. Mass spectrometric determination of aspartame decomposition products. Evidence for β‐isomer formation in solution. Food Additives & Contaminants. 1989;6(4):397–414. https://doi.org/10.1080/02652038909373799

12. Qin X.-Z. Atmospheric pressure chemical ionization tandem mass spectra of α- and β-aspartame. Journal of Massspectrometry. 1998;33(1):55–63. https://doi.org/10.1002/(SICI)1096–9888(199801)33:13.0.CO;2-A.