Improvement of the State Primary Standard in the Field of Organic Analysis GET 208

In the context of the rapid development of the Russian pharmaceutical industry, there is an urgent need to improve the State Primary Standard for the 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).

As a result of the improvement of GET 208 carried out in 2023, a new installation based on the highperformance liquid chromatography/high-resolution mass spectrometry method was included in the standard. Thus, the functionality of the GPE was expanded in accordance with the current requirements of the domestic industry and for the purpose of Russia’s successful participation in international comparisons in the field of organic analysis now and in the medium term.

The article presents materials on the study of the capabilities of the new installation for solving various measurement problems in the field of organic analysis, describes specific analytical techniques and measurement methods, and provides experimental data and summarized results. Based on the completed studies, the metrological characteristics of GET 208 have been improved in terms of reproducing units of mass (molar) fraction of the main component in pure organic substances, mass fraction of organic components in solutions and materials.

Improvement of GET 208 made it possible to create a scientific, methodological and instrumental basis for reproducing measurement units for a wide range of organic compounds.

1. Kaarls R., Quinn T. J. The Comite Consultatif pour la Quantite de Matiere: a brief review of its origin and present activities. Metrologia. 1997;34(1):1–5. http://iopscience.iop.org/0026–1394/34/1/1

2. Westwood S., Lippa K., Shimuzu Y., Lalerle B., Saito T., Duewer D. et al. Methods for the SI-traceable value assignment of the purity of organic compounds (IUPAC Technical Report). Pure and Applied Chemistry. 2023;95(1):1–77. https://doi.org/10.1515/pac-2020–0804

3. 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

4. Lippa K. A., Duewer D. L., Nelson M. A., Davies S. R., Mackay L. G. The role of the CCQM OAWG in providing SI traceable calibrators for organic chemical measurements. Accreditation and Quality Assurance. 2019;24:407–415. https://doi.org/10.1007/s00769-019-01407-6

5. Mikheeva A. Yu., Krylov A. I. Traceability in organic analysis. Report 1: Equivalence of the national and international measurement standards. Measurement Standards. Reference Materials. 2020;16(3):5–21. (In Russ.). https://doi.org/10.20915/2687-0886-2020-16-3-5-21

6. International System of Units (SI): Federal Agency for Technical Regulation and Metrology. 9th ed. Moscow: Rosstandart; 2019. 100 p. (In Russ.).

7. Milman B. L., Zhurkovich I. K. Summarized criteria of chemical compounds identification by chromatographymass spectrometry. Analytics and control. 2020;24(3):164–173. (In Russ.). https://elar.urfu.ru/handle/10995/97975

8. Granados-Chinchilla F., Rodriguez C. Tetracyclines in food and feedingstuffs: from regulation to analytical methods, bacterial resistance, and environmental and health implications. Journal of Analytical Methods in Chemistry. 2017;2017:1–24. https://doi.org/10.1155/2017/1315497

9. Lykkeberg A. K., Halling-Sorensen B., Cornett C., Tjornelund J., Honore Hansen S. Quantitative analysis of oxytetracycline and its impurities by LC–MS-MS. Journal of Pharmaceutical and Biomedical Analysis. 2004;34(2):325–332. https://doi.org/10.1016/S0731–7085(03)00500-4

10. Granja R. H. M. M., Nino A. M. M., Reche K. V. G., Giannotti F. M., de Lima A. C., Wanschel A. C. B. A. et al. Determination and confirmation of metronidazole, dimetridazole, ronidazole and their metabolites in bovine muscle by LC–MS/MS. Food Additives & Contaminants: Part A. 2013;30(6):970–976. http://dx.doi.org/10.1080/19440049.2013.787653

11. Hajrulai-Musliu Z., Uzunov R., Jovanov S., Jankuloski D., Stojkovski V., Pendovski L. et al. A new LC–MS/MS method for multiple residues/contaminants in bovine meat. BMC Chemistry. 2021;15(1):62. https://doi.org/10.1186/s13065-021-00788-5

12. Chen D., Delmas J. M., Hurtaud-Pessel D., Verdon E. Development of a multi-class method to determine nitroimidazoles, nitrofurans, pharmacologically active dyes and chloramphenicol in aquaculture products by liquid chromatography-tandem mass spectrometry. Food Chemistry. 2020;311:125924. https://doi.org/10.1016/j.foodchem.2019.125924