Gas chromatographic determination of methylsulfonylmethane in an anti-arthritic combined pharmaceutical product

Authors

DOI:

https://doi.org/10.15587/2519-4852.2026.353242

Keywords:

methylsulfonylmethane, gas chromatography, GC-MS, GC-FID, validation of analytical methods, pharmaceutical analysis, combination medicinal product, quality control, quantification

Abstract

Methylsulfonylmethane is a pharmacologically active compound that is widely used in mono- and combined pharmaceutical preparations to maintain the functional state of the musculoskeletal system. The development of promising anti-arthritic drugs requires proper analytical support, particularly the use of validated methods suitable for routine quality control in accordance with modern pharmaceutical requirements.

The aim. The aim of the study was to develop and validate methods for the quantitative determination of methylsulfonylmethane in a combined medicinal product using gas chromatography with mass-selective detection (GC-MS) and flame ionization detection (GC-FID), and to compare their validation characteristics.

Materials and methods. The object of the study was a combined medicinal product in the form of a powder containing methylsulfonylmethane, glucosamine sulfate, chondroitin sulfate sodium and excipients. The study was conducted using Shimadzu GC/MS GCMS-QP2020 EI and Shimadzu GC-2010 Plus AF gas chromatographs with a flame ionization detector using capillary columns of type 5MS and the external standard method. The validation of the methods was carried out in accordance with the requirements of the State Pharmacopoeia of Ukraine and ICH Q2(R1) recommendations.

Results. Two methods for the identification and quantitative determination of methylsulfonylmethane by gas chromatography were developed. The retention time of MSM by the GC-MS method was 9.157 min in the reference solution and 9.163 min in the test solution, and by the GC-FID method - 8.456 and 8.442 min, respectively. The validation characteristics of the methods were confirmed in the range of 80–120% of the nominal content (0.32–0.48 mg/ml) with correlation coefficients r > 0.9981. The relative standard deviations did not exceed 0.42%, and the total analytical uncertainty met the pharmacopoeial acceptance criteria

Conclusions. The proposed methods are accurate, reproducible and suitable for routine quality control of combination medicinal products containing methylsulfonylmethane

Author Biographies

Andrii Koptielov, National University of Pharmacy

PhD Student

Department of Pharmaceutical Chemistry

Volodymyr Petruk, Transcarpathian Research Expert Forensic Center of the Ministry of Internal Affairs of Ukraine

Head of Department

Materials, Substances and Products Research Department

Olena Bevz, National University of Pharmacy

PhD, Associate Professor

Department of Pharmaceutical Chemistry

Olha Rudakova, Фаховий коледж Національного фармацевтичного університету

PhD, Lecturer

Cyclic Committee of Pharmaceutical Chemistry and Pharmacognosy

Oleksandr Kryvanych, State Institution of Higher Education “Uzhhorod National University”

PhD, Associate Professor

Department of Pharmaceutical Disciplines

Nataliia Bevz, National University of Pharmacy

PhD, Associate Professor

Department of Pharmaceutical Chemistry

Yaroslav Studenyak, State Institution of Higher Education “Uzhhorod National University”

PhD, Associate Professor, Head of Department

Department of Analytical Chemistry

References

  1. Bloomer, R. J., Butawan, M., Lin, L., Ma, D., Yates, C. R. (2019). Blood MSM Concentrations Following Escalating Dosages Of Oral MSM In Men And Women. Journal of Nutrition & Food Sciences, 9 (1). https://doi.org/10.4172/2155-9600.1000748
  2. Colletti, A., Cicero, A. F. G. (2021). Nutraceutical Approach to Chronic Osteoarthritis: From Molecular Research to Clinical Evidence. International Journal of Molecular Sciences, 22 (23), 12920. https://doi.org/10.3390/ijms222312920
  3. Toguchi, A., Noguchi, N., Kanno, T., Yamada, A. (2023). Methylsulfonylmethane Improves Knee Quality of Life in Participants with Mild Knee Pain: A Randomized, Double-Blind, Placebo-Controlled Trial. Nutrients, 15 (13), 2995. https://doi.org/10.3390/nu15132995
  4. Kim, L. S., Axelrod, L. J., Howard, P., Buratovich, N., Waters, R. F. (2006). Efficacy of methylsulfonylmethane (MSM) in osteoarthritis pain of the knee: a pilot clinical trial. Osteoarthritis and Cartilage, 14 (3), 286–294. https://doi.org/10.1016/j.joca.2005.10.003
  5. Global, regional, and national burden of osteoarthritis, 1990–2020 and projections to 2050: A systematic analysis for the Global Burden of Disease Study 2021 (2023). The Lancet Rheumatology, 5 (9), e508–e522. Available at: https://www.thelancet.com/journals/lanrhe/article/PIIS2665-9913(23)00163-7/fulltext
  6. Brough, L., Rees, G., Drummond-Clarke, L., McCallum, J. E., Taylor, E., Kozhevnikov, O., Walker, S. (2025). Can Dietary Supplements Support Muscle Function and Physical Activity? A Narrative Review. Nutrients, 17 (21), 3495. https://doi.org/10.3390/nu17213495
  7. Butawan, M., Benjamin, R., Bloomer, R. (2017). Methylsulfonylmethane: Applications and Safety of a Novel Dietary Supplement. Nutrients, 9 (3), 290. https://doi.org/10.3390/nu9030290
  8. Koptielov, A. S., Deineka, A. S., Bevz, N. Yu., Kukhtenko, O. S. (2024). Determination of pharmacotechnological parameters of active pharmaceutical ingredients in the development of a chondroprotective medicine. Health & Education, 1, 99–104. https://doi.org/10.32782/health-2024.1.13
  9. Belikova, A., Materienko, A., Sidorenko, L., Chornyi, V., Korzh, I., Kucherenko, L. et al. (2022). Development of a method for determining the morpholinium thiazotate using more economic and green GC/MS assay with an fid detector. ScienceRise: Pharmaceutical Science, 3 (37), 4–11. https://doi.org/10.15587/2519-4852.2022.259879
  10. Dietary Supplement Monographs, Methylsulfonylmethane. USP-NF (2019). Rockville: United States Pharmacopeia. https://doi.org/10.31003/USPNF_M53000_04_01
  11. Dietary Supplement Monographs, Methylsulfonylmethane Tablets. USP-NF (2017). Rockville: United States Pharmacopeia. https://doi.org/10.31003/USPNF_M2187_01_01
  12. Dietary Supplement Monographs, Glucosamine, Chondroitin Sulfate Sodium, and Methylsulfonylmethane Tablets. USP-NF (2017). Rockville: United States Pharmacopeia. https://doi.org/10.31003/USPNF_M2189_01_01
  13. Dietary Supplement Monographs, Glucosamine and Methylsulfonylmethane Tablets. USP-NF (2017). Rockville: United States Pharmacopeia. https://doi.org/10.31003/USPNF_M2188_01_01
  14. Derzhavna Farmakopeia Ukrainy. Dopovnennia 7. Vol. 2 (2024). Kharkiv: Derzhavne pidpryiemstvo «Ukrainskyi naukovyi farmakopeinyi tsentr yakosti likarskykh zasobiv», 424.
  15. Dejaegher, B., Smeyers-Verbeke, J., Vander Heyden, Y.; Poole, C. F. (Ed.) (2021). Validation of gas chromatographic methods. Gas Chromatography. Elsevier, 547–560. https://doi.org/10.1016/B978-0-12-820675-1.00027-7
  16. ICH Q2(R1) – Validation of Analytical Procedures: Text and Methodology (2005). International Council for Harmonisation.
  17. Kozhuharov, V. R., Ivanov, K., Karcheva-Bahchevanska, D., Prissadova, N., Ivanova, S. (2023). Development and Validation of Gas Chromatography–Mass Spectrometry Method for Quantification of Sibutramine in Dietary Supplements. Processes, 11 (8), 2337. https://doi.org/10.3390/pr11082337
  18. Cherniakova, V., Myhal, A., Rudiuk, V., Kryvanych, O., Rudakova, O., Tugaibei, I. et al. (2024). Determination of chromatographic conditions for quantitative assessment of active components in complex nasal spray after manufacturing and expiry date. ScienceRise: Pharmaceutical Science, 1 (47), 30–39. https://doi.org/10.15587/2519-4852.2024.299184
  19. Harmita, H., Hayun, H., Geofani, M. H. (2020). Quantification of hyaluronic acid and methylsulfonylmethane in dietary supplements. International Journal of Applied Pharmaceutics, 12 (1), 143–148. https://doi.org/10.22159/ijap.2020.v12s1.ff032
  20. Šatínský, D., Pospíšilová, M., Sladkovský, R. (2013). A New Gas Chromatography Method for Quality Control of Methylsulfonylmethane Content in Multicomponent Dietary Supplements. Food Analytical Methods, 7 (5), 1118–1122. https://doi.org/10.1007/s12161-013-9722-5
  21. Zhong, Z., Chen, Y., Xia, H., Chen, Z., Cheng, Q. (2021). Development and Validation of a Sensitive GC–MS/MS Method for the Determination of Five Potential Genotoxic Impurities in Abiraterone Acetate. Journal of Chromatographic Science, 60 (2), 105–110. https://doi.org/10.1093/chromsci/bmab052
Gas chromatographic determination of methylsulfonylmethane in an anti-arthritic combined pharmaceutical product

Downloads

Published

2026-02-28

How to Cite

Koptielov, A., Petruk, V. ., Bevz, O., Rudakova, O., Kryvanych, O., Bevz, N., & Studenyak, Y. (2026). Gas chromatographic determination of methylsulfonylmethane in an anti-arthritic combined pharmaceutical product. ScienceRise: Pharmaceutical Science, (1 (59), 91–99. https://doi.org/10.15587/2519-4852.2026.353242

Issue

Section

Pharmaceutical Science