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

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