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Determination of Methyl Methanesulfonate and Ethyl Methanesulfonate in Methanesulfonic Acid by Derivatization Followed by High-Performance Liquid Chromatography With Ultraviolet Detection

Jie Zhou, Jie Xu, Xiangyuan Zheng, Wenyuan Liu, Feng Zheng

J Sep Sci. 2017 Sep;40(17):3414-3421.

PMID: 28675589

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.

Chemicals Related in the Paper:

Catalog Number Product Name Structure CAS Number Price
AP62500 Ethyl methanesulfonate Ethyl methanesulfonate 62-50-0 Price
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