Methylsulfonylmethane DEFINITION Methylsulfonylmethane contains NLT 98.0% and NMT 102.0% of methylsulfonylmethane (C2H6O2S), calculated on the anhydrous basis. The chromatographic purity is NLT 99.8%. IDENTIFICATION • B. The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay. ASSAY • Procedure Diluent: Transfer 950 mL of methanol to a 1-L volumetric flask. Add 0.60 mL of di(ethylene glycol) methyl ether, and dilute with methanol to volume. Standard solution: 0.4 mg/mL of USP Methylsulfonylmethane RS in Diluent. Sonicate at 50 for 1 min, and allow to cool to room temperature. Sample solution: 0.4 mg/mL of Methylsulfonylmethane in Diluent. Sonicate at 50 for 1 min, and allow to cool to room temperature. Chromatographic system Mode: GC Detector: Flame ionization Column: 0.53-mm × 30-m capillary column coated with a 5-µm phase G2 Temperature Column: 120 Injector: 250 Detector: 250 Carrier gas: Helium Flow rate: 5 mL/min Split ratio: 2:1 Injection size: 1 µL System suitability Sample: Standard solution Suitability requirements Relative standard deviation: NMT 2.0% for the peak response ratio of methylsulfonylmethane to di(ethylene glycol) methyl ether from replicate injections Analysis Samples: Standard solution and Sample solution Calculate the percentage of methylsulfonylmethane (C2H6O2S) in the portion of Methylsulfonylmethane taken: Result = (RU/RS) × (CS/CU) × 100
Acceptance criteria: 98.0%102.0% on the anhydrous basis IMPURITIES • Heavy Metals, Method I 231: NMT 3 µg/g • Chromatographic Purity and Limit of Dimethyl Sulfoxide Standard stock solution: 1.0 mg/mL of USP Dimethyl Sulfoxide RS in methanol Sensitivity check solution: 2.0 µg/mL from the Standard stock solution in methanol System suitability solution: 0.1 mg/mL of USP Dimethyl Sulfoxide RS and 0.4 mg/mL of USP Methylsulfonylmethane RS in methanol. In a 50-mL volumetric flask dissolve 20 mg of USP Methylsulfonylmethane RS in 5 mL of the Standard stock solution, and dilute with methanol to volume. Sample solution: 2 mg/mL of Methylsulfonylmethane in methanol. Sonicate at 50 for 1 min, and allow to cool to room temperature. Chromatographic system: Proceed as directed in the Assay. System suitability Samples: Sensitivity check solution and System suitability solution Suitability requirements Signal-to-noise ratio: NLT 10 for dimethyl sulfoxide peak, Sensitivity check solution Resolution: NLT 2.0 between dimethyl sulfoxide and methylsulfonylmethane, System suitability solution Analysis Sample: Sample solution Calculate the percentage of each impurity in the portion of Methylsulfonylmethane taken: Result = (rU/rT) × 100
Acceptance criteria Individual impurities: NMT 0.1% of dimethyl sulfoxide; NMT 0.05% of any other individual impurity Total impurities: NMT 0.2% for all impurities, including dimethyl sulfoxide SPECIFIC TESTS • Melting Range or Temperature 741: 108.5110.5 • Microbial Enumeration Tests 2021: The total aerobic microbial count is NMT 103 cfu/g or mL, and the total combined molds and yeasts count is NMT 102 cfu/g or mL. • Absence of Specified Microorganisms 2022: It meets the requirements for absence of Escherichia coli in 10 g. • Water Determination, Method I 921: NMT 0.1%. [Note500 mg of methylsulfonylmethane may be required for this analysis. ] ADDITIONAL REQUIREMENTS • Packaging and Storage: Preserve in well-closed containers. • USP Reference Standards 11 USP Methylsulfonylmethane RS Dimethyl sulfone. C2H6O2S 94.13 Auxiliary Information Please check for your question in the FAQs before contacting USP.
USP35NF30 Page 1383 Pharmacopeial Forum: Volume No. 32(3) Page 826Chromatographic Column Chromatographic columns text is not derived from, and not part of, USP 35 or NF 30. |