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- Title
Determination of methyl methanesulfonate and ethyl methanesulfonate in methanesulfonic acid by derivatization followed by high-performance liquid chromatography with ultraviolet detection.
- Authors
Zhou, Jie; Xu, Jie; Zheng, Xiangyuan; Liu, Wenyuan; Zheng, Feng
- Abstract
Methanesulfonic acid is routinely used in pharmaceuticals but can contain potentially genotoxic impurities such as methyl methanesulfonate and ethyl methanesulfonate. The aim of this study was to develop a simple high-performance liquid chromatography with ultraviolet detection method for determining methyl methanesulfonate and ethyl methanesulfonate in methanesulfonic acid. Samples (250 mg) in water/acetonitrile (200 μL) were first combined with 10.0 mol/L sodium hydroxide solution (270 μL). Then they were mixed with 2.0 mg/mL N, N-diethyldithiocarbamate (500 μL), diluted to 5 mL with N, N-dimethylacetamide and allowed to react at 80°C for 1 h. The derivatives were analyzed using gradient high-performance liquid chromatography with ultraviolet detection (277 nm) and structurally elucidated by liquid chromatography with mass spectrometry. With acetonitrile/5 mmol/L ammonium acetate solution as the eluent and 1 mL/min as the flow rate on a C18 column, the derivatives were eluted at 10.6 and 14.8 min. Good linearity (correlation coefficients > 0.999) and low limits of quantitation (0.6 ppm) were obtained. The recoveries were in the range of 80-115% with relative standard deviation < 5.0%. Finally, the established method was successfully used for the determination of methyl methanesulfonate and ethyl methanesulfonate in methanesulfonic acid.
- Subjects
GENETIC toxicology; DERIVATIZATION; DIETHYLDITHIOCARBAMATE; METHANESULFONATES; METHYL methanesulfonate
- Publication
Journal of Separation Science, 2017, Vol 40, Issue 17, p3414
- ISSN
1615-9306
- Publication type
Article
- DOI
10.1002/jssc.201700543